Spectroscopic analysis of hot-water- and dilute-acid-extracted hardwood and softwood chips

NASA Astrophysics Data System (ADS)

Lehto, Joni; Louhelainen, Jarmo; Huttunen, Marko; Alén, Raimo

2017-09-01

Hot-water and dilute sulfuric acid pretreatments were performed prior to chemical pulping for silver/white birch (Betula pendula/B. pubescens) and Scots pine (Pinus sylvestris) chips to determine if varying pretreatment conditions on the original wood material were detectable via attenuated total reflectance (ATR) infrared spectroscopy. Pretreatment conditions varied with respect to temperature (130 °C and 150 °C) and treatment time (from 30 min to 120 min). The effects of the pretreatments on the composition of wood chips were determined by ATR infrared spectroscopy. The spectral data were compared to those determined by common wood chemistry analyses to evaluate the suitability of ATR spectroscopy method for rapid detection of changes in the wood chemical composition caused by different pretreatment conditions. In addition to determining wood species-dependent differences in the wood chemical composition, analytical results indicated that most essential lignin- and carbohydrates-related phenomena taking place during hot-water and acidic pretreatments could be described by applying this simple spectral method requiring only a small sample amount and sample preparation. Such information included, for example, the cleavage of essential lignin bonds (i.e., mainly β-O-4 linkages in guaiacyl and syringyl lignin) and formation of newly condensed lignin structures under different pretreatment conditions. Carbohydrate analyses indicated significant removal of hemicelluloses (especially hardwood xylan) and hemicelluloses-derived acetyl groups during the pretreatments, but they also confirmed the highly resistant nature of cellulose towards mild pretreatments.

Spectroscopic analysis of hot-water- and dilute-acid-extracted hardwood and softwood chips.

PubMed

Lehto, Joni; Louhelainen, Jarmo; Huttunen, Marko; Alén, Raimo

2017-09-05

Hot-water and dilute sulfuric acid pretreatments were performed prior to chemical pulping for silver/white birch (Betula pendula/B. pubescens) and Scots pine (Pinus sylvestris) chips to determine if varying pretreatment conditions on the original wood material were detectable via attenuated total reflectance (ATR) infrared spectroscopy. Pretreatment conditions varied with respect to temperature (130°C and 150°C) and treatment time (from 30min to 120min). The effects of the pretreatments on the composition of wood chips were determined by ATR infrared spectroscopy. The spectral data were compared to those determined by common wood chemistry analyses to evaluate the suitability of ATR spectroscopy method for rapid detection of changes in the wood chemical composition caused by different pretreatment conditions. In addition to determining wood species-dependent differences in the wood chemical composition, analytical results indicated that most essential lignin- and carbohydrates-related phenomena taking place during hot-water and acidic pretreatments could be described by applying this simple spectral method requiring only a small sample amount and sample preparation. Such information included, for example, the cleavage of essential lignin bonds (i.e., mainly β-O-4 linkages in guaiacyl and syringyl lignin) and formation of newly condensed lignin structures under different pretreatment conditions. Carbohydrate analyses indicated significant removal of hemicelluloses (especially hardwood xylan) and hemicelluloses-derived acetyl groups during the pretreatments, but they also confirmed the highly resistant nature of cellulose towards mild pretreatments. Copyright © 2017 Elsevier B.V. All rights reserved.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

PubMed Central

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-01-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples. PMID:27924944

Characterization of halogenated DBPs and identification of new DBPs trihalomethanols in chlorine dioxide treated drinking water with multiple extractions.

PubMed

Han, Jiarui; Zhang, Xiangru; Liu, Jiaqi; Zhu, Xiaohu; Gong, Tingting

2017-08-01

Chlorine dioxide (ClO 2 ) is a widely used alternative disinfectant due to its high biocidal efficiency and low-level formation of trihalomethanes and haloacetic acids. A major portion of total organic halogen (TOX), a collective parameter for all halogenated DBPs, formed in ClO 2 -treated drinking water is still unknown. A commonly used pretreatment method for analyzing halogenated DBPs in drinking water is one-time liquid-liquid extraction (LLE), which may lead to a substantial loss of DBPs prior to analysis. In this study, characterization and identification of polar halogenated DBPs in a ClO 2 -treated drinking water sample were conducted by pretreating the sample with multiple extractions. Compared to one-time LLE, the combined four-time LLEs improved the recovery of TOX by 2.3 times. The developmental toxicity of the drinking water sample pretreated with the combined four-time LLEs was 1.67 times higher than that pretreated with one-time LLE. With the aid of ultra-performance liquid chromatography/electrospray ionization-triple quadrupole mass spectrometry, a new group of polar halogenated DBPs, trihalomethanols, were detected in the drinking water sample pretreated with multiple extractions; two of them, trichloromethanol and bromodichloromethanol, were identified with synthesized standard compounds. Moreover, these trihalomethanols were found to be the transformation products of trihalomethanes formed during ClO 2 disinfection. The results indicate that multiple LLEs can significantly improve extraction efficiencies of polar halogenated DBPs and is a better pretreatment method for characterizing and identifying new polar halogenated DBPs in drinking water. Copyright © 2017. Published by Elsevier B.V.

Ultraviolet resonance Raman spectroscopy for the detection of cocaine in oral fluid

NASA Astrophysics Data System (ADS)

D'Elia, Valentina; Montalvo, Gemma; Ruiz, Carmen García; Ermolenkov, Vladimir V.; Ahmed, Yasmine; Lednev, Igor K.

2018-01-01

Detecting and quantifying cocaine in oral fluid is of significant importance for practical forensics. Up to date, mainly destructive methods or biochemical tests have been used, while spectroscopic methods were only applied to pretreated samples. In this work, the possibility of using resonance Raman spectroscopy to detect cocaine in oral fluid without pretreating samples was tested. It was found that ultraviolet resonance Raman spectroscopy with 239-nm excitation allows for the detection of cocaine in oral fluid at 10 μg/mL level. Further method development will be needed for reaching the practically useful levels of cocaine detection.

Synergy of Siam weed (Chromolaena odorata) and poultry manure for energy generation: Effects of pretreatment methods, modeling and process optimization.

PubMed

Dahunsi, S O; Oranusi, S; Owolabi, J B; Efeovbokhan, V E

2017-02-01

The co-digestion of Chromolaena odorata with poultry manure was evaluated in this study. Two samples of the weed: (A: which was pre-treated with mechanical, chemical and thermal methods) and (B: which was pretreated using mechanical and chemical methods only) were separately digested with poultry manure. Biogas generation started from the 2nd to 4th and 4th to 7th day for samples 'A' and 'B' respectively. The most desired actual biogas yield from samples 'A' and 'B' were 3884.20 and 2544.70 (10 -4 m 3 /kg VS) respectively and the gas composition was 68±2% Methane and 20±2% Carbon dioxide for sample A while it was 62±3% Methane and 22±2% Carbon dioxide for sample B. In all, there was a 38.06% increase in gas generation in 'A' over 'B'. The coefficient of determination (R 2 ) for the Response Surface Methodology (RSM) model (0.9009) was high suggesting high accuracy in the modeling and prediction. The worldwide usage of C. odorata is encouraged. Copyright © 2016 Elsevier Ltd. All rights reserved.

Pretreatment of Oil Palm Frond (OPF) with Ionic Liquid

NASA Astrophysics Data System (ADS)

Azmi, I. S.; Azizan, A.; Salleh, R. Mohd

2018-05-01

Pretreatment is the key to unlock the recalcitrance of lignocellulose for cellulosic biofuel production. Increasing attention has been drawn to ionic liquids (ILs) for pretreatment of lignocellulosic biomass because this approach was considered as a green engineering method over other conventional methods. In this work, Oil palm frond (OPF) was pretreated by using the ionic liquid 1-ethyl-3-methylimidazolium acetate [EMIM] Ac at the temperature of 99˚C for 3 hours. The characterization of the untreated and pretreated OPF was conducted by using different techniques which are Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The pretreatment of OPF with [EMIM] Ac was demonstrated to be effective evidenced by the significant reduction of Lateral Order Index (LOI) from FTIR, reduction of Crystallinity Index (CI) based on XRD and the significant morphology changes indicated by SEM. The CI value for the pretreated OPF decreased from 0.47 (untreated sample) to 0.28 while the LOI value decreased from 1.10 to 0.24 after pretreatment with [EMIM]Ac and the SEM morphology showed that the pretreated OPF becomes distorted and disordered.

Quantification and characterisation of fatty acid methyl esters in microalgae: Comparison of pretreatment and purification methods.

PubMed

Lage, Sandra; Gentili, Francesco G

2018-06-01

A systematic qualitative and quantitative analysis of fatty acid methyl esters (FAMEs) is crucial for microalgae species selection for biodiesel production. The aim of this study is to identify the best method to assess microalgae FAMEs composition and content. A single-step method, was tested with and without purification steps-that is, separation of lipid classes by thin-layer chromatography (TLC) or solid-phase extraction (SPE). The efficiency of a direct transesterification method was also evaluated. Additionally, the yield of the FAMEs and the profiles of the microalgae samples with different pretreatments (boiled in isopropanol, freezing, oven-dried and freeze-dried) were compared. The application of a purification step after lipid extraction proved to be essential for an accurate FAMEs characterisation. The purification methods, which included TLC and SPE, provided superior results compared to not purifying the samples. Freeze-dried microalgae produced the lowest FAMEs yield. However, FAMEs profiles were generally equivalent among the pretreatments. Copyright © 2018 Elsevier Ltd. All rights reserved.

Pretreatment of whole blood using hydrogen peroxide and UV irradiation. Design of the advanced oxidation process.

PubMed

Bragg, Stefanie A; Armstrong, Kristie C; Xue, Zi-Ling

2012-08-15

A new process to pretreat blood samples has been developed. This process combines the Advanced Oxidation Process (AOP) treatment (using H(2)O(2) and UV irradiation) with acid deactivation of the enzyme catalase in blood. A four-cell reactor has been designed and built in house. The effect of pH on the AOP process has been investigated. The kinetics of the pretreatment process shows that at high C(H(2)O(2),t=0), the reaction is zeroth order with respect to C(H(2)O(2)) and first order with respect to C(blood). The rate limiting process is photon flux from the UV lamp. Degradation of whole blood has been compared with that of pure hemoglobin samples. The AOP pretreatment of the blood samples has led to the subsequent determination of chromium and zinc concentrations in the samples using electrochemical methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of mechanical disruption on the effectiveness of three reactors used for dilute acid pretreatment of corn stover Part 1: chemical and physical substrate analysis

PubMed Central

2014-01-01

Background There is considerable interest in the conversion of lignocellulosic biomass to liquid fuels to provide substitutes for fossil fuels. Pretreatments, conducted to reduce biomass recalcitrance, usually remove at least some of the hemicellulose and/or lignin in cell walls. The hypothesis that led to this research was that reactor type could have a profound effect on the properties of pretreated materials and impact subsequent cellulose hydrolysis. Results Corn stover was dilute-acid pretreated using commercially relevant reactor types (ZipperClave® (ZC), Steam Gun (SG) and Horizontal Screw (HS)) under the same nominal conditions. Samples produced in the SG and HS achieved much higher cellulose digestibilities (88% and 95%, respectively), compared to the ZC sample (68%). Characterization, by chemical, physical, spectroscopic and electron microscopy methods, was used to gain an understanding of the effects causing the digestibility differences. Chemical differences were small; however, particle size differences appeared significant. Sum-frequency generation vibrational spectra indicated larger inter-fibrillar spacing or randomization of cellulose microfibrils in the HS sample. Simons’ staining indicated increased cellulose accessibility for the SG and HS samples. Electron microscopy showed that the SG and HS samples were more porous and fibrillated because of mechanical grinding and explosive depressurization occurring with these two reactors. These structural changes most likely permitted increased cellulose accessibility to enzymes, enhancing saccharification. Conclusions Dilute-acid pretreatment of corn stover using three different reactors under the same nominal conditions gave samples with very different digestibilities, although chemical differences in the pretreated substrates were small. The results of the physical and chemical analyses of the samples indicate that the explosive depressurization and mechanical grinding with these reactors increased enzyme accessibility. Pretreatment reactors using physical force to disrupt cell walls increase the effectiveness of the pretreatment process. PMID:24713111

The potential value of the seaweed Ceylon moss (Gelidium amansii) as an alternative bioenergy resource.

PubMed

Wi, Seung Gon; Kim, Hyun Joo; Mahadevan, Shobana Arumugam; Yang, Duck-Joo; Bae, Hyeun-Jong

2009-12-01

Sea weed (Ceylon moss) possesses comparable bioenergy production potential to that of land plants. Ceylon moss has high content of carbohydrates, typically galactose (23%) and glucose (20%). We have explored the possibility of sodium chlorite in Ceylon moss pretreatment that can ultimately increase the efficiency of enzymatic saccharification. In an acidic medium, chlorite generates ClO(2) molecules that transform lignin into soluble compounds without any significant loss of carbohydrate content and this procedure is widely used as an analytical method for holocellulose determination. Sodium chlorite-pretreated samples resulted in glucose yield up to 70% with contrast of only 5% was obtained from non-pretreated samples. The efficiency of enzymatic hydrolysis is significantly improved by sodium chlorite pretreatment, and thus sodium chlorite pretreatment is potentially a very useful tool in the utilisation of Ceylon moss biomass for ethanol production or bioenergy purposes.

Evaluation of Biological Pretreatment of Rubberwood with White Rot Fungi for Enzymatic Hydrolysis

PubMed Central

Nazarpour, Forough; Abdullah, Dzulkefly Kuang; Abdullah, Norhafizah; Zamiri, Reza

2013-01-01

The effects of biological pretreatment on the rubberwood (Hevea brasiliensis), was evaluated after cultivation of white rot fungi Ceriporiopsis subvermispora, Trametes versicolor, and a mixed culture of C. subvermispora and T. versicolor. The analysis of chemical compositions indicated that C. subvermispora had greater selectivity for lignin degradation with the highest lignin and hemicellulose loss at 45.06% and 42.08%, respectively, and lowest cellulose loss (9.50%) after 90 days among the tested samples. X-ray analysis showed that pretreated samples had a higher crystallinity than untreated samples. The sample pretreated by C. subvermispora presented the highest crystallinity of all the samples which might be caused by the selective degradation of amorphous components. Fourier transform infrared (FT-IR) spectroscopy demonstrated that the content of lignin and hemicellulose decreased during the biological pretreatment process. A study on hydrolysis of rubberwood treated with C. subvermispora, T. versicolor, and mixed culture for 90 days resulted in an increased sugar yield of about 27.67%, 16.23%, and 14.20%, respectively, as compared with untreated rubberwood (2.88%). The results obtained demonstrate that rubberwood is a potential raw material for industrial applications and white rot fungus C. subevermispora provides an effective method for improving the enzymatic hydrolysis of rubberwood. PMID:28809260

Comparison of pretreatment methods on the enzymatic Saccharification of aspen wood

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pinto, J.H.; Kamden, D.P.

Five different chemical pretreatments, using dilute sulfuric acid, sodium hydroxide, hydrogen peroxide and sodium hydroxide, peroxy-monosulfate, and acetic acid, were applied to aspen thermomechanical fibers. The pretreated fibers were submitted to enzymatic hydrolysis and the liberated glucose was monitored. High glucose concentrations were observed for the peroxymonosulfate and the acetic acid pretreated samples. Glucose concentrations greater than 25 g/L were obtained in these cases. This corresponds to conversions on the order of 90% of the retreated substrate glucose content. 18 refs., 1 fig., 4 tabs.

Atmospheric corrosion of metals in industrial city environment.

PubMed

Kusmierek, Elzbieta; Chrzescijanska, Ewa

2015-06-01

Atmospheric corrosion is a significant problem given destruction of various materials, especially metals. The corrosion investigation in the industrial city environment was carried out during one year exposure. Corrosion potential was determined using the potentiometric method. The highest effect of corrosion processes was observed during the winter season due to increased air pollution. Corrosion of samples pre-treated in tannic acid before the exposure was more difficult compared with the samples without pretreatment. The corrosion products determined with the SEM/EDS method prove that the most corrosive pollutants present in the industrial city air are SO2, CO2, chlorides and dust.

Evaluation of the direct and diffusion methods for the determination of fluoride content in table salt

PubMed Central

Martínez-Mier, E. Angeles; Soto-Rojas, Armando E.; Buckley, Christine M.; Margineda, Jorge; Zero, Domenick T.

2010-01-01

Objective The aim of this study was to assess methods currently used for analyzing fluoridated salt in order to identify the most useful method for this type of analysis. Basic research design Seventy-five fluoridated salt samples were obtained. Samples were analyzed for fluoride content, with and without pretreatment, using direct and diffusion methods. Element analysis was also conducted in selected samples. Fluoride was added to ultra pure NaCl and non-fluoridated commercial salt samples and Ca and Mg were added to fluoride samples in order to assess fluoride recoveries using modifications to the methods. Results Larger amounts of fluoride were found and recovered using diffusion than direct methods (96%–100% for diffusion vs. 67%–90% for direct). Statistically significant differences were obtained between direct and diffusion methods using different ion strength adjusters. Pretreatment methods reduced the amount of recovered fluoride. Determination of fluoride content was influenced both by the presence of NaCl and other ions in the salt. Conclusion Direct and diffusion techniques for analysis of fluoridated salt are suitable methods for fluoride analysis. The choice of method should depend on the purpose of the analysis. PMID:20088217

The effect of alkaline pretreatment methods on cellulose structure and accessibility

DOE PAGES

Bali, Garima; Meng, Xianzhi; Deneff, Jacob I.; ...

2014-11-24

The effects of different alkaline pretreatments on cellulose structural features and accessibility are compared and correlated with the enzymatic hydrolysis of Populus. The pretreatments are shown to modify polysaccharides and lignin content to enhance the accessibility for cellulase enzymes. The highest increase in the cellulose accessibility was observed in dilute sodium hydroxide, followed by methods using ammonia soaking and lime (Ca(OH) 2). The biggest increase of cellulose accessibility occurs during the first 10 min of pretreatment, with further increases at a slower rate as severity increases. Low temperature ammonia soaking at longer residence times dissolved a major portion of hemicellulosemore » and exhibited higher cellulose accessibility than high temperature soaking. Moreover, the most significant reduction of degree of polymerization (DP) occurred for dilute sodium hydroxide (NaOH) and ammonia pretreated Populus samples. The study thus identifies important cellulose structural features and relevant parameters related to biomass recalcitrance.« less

Comparison of ion chromatographic methods based on conductivity detection, post-column-reaction and on-line-coupling IC-ICP-MS for the determination of bromate.

PubMed

Schminke, G; Seubert, A

2000-02-01

An established method for the determination of the disinfection by-product bromate is ion chromatography (IC). This paper presents a comparison of three IC methods based on either conductivity detection (IC-CD), a post-column-reaction (IC-PCR-VIS) or the on-line-coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS). Main characteristics of the methods such as method detection limits (MDL), time of analysis and sample pretreatment are compared and applicability for routine analysis is critically discussed. The most sensitive and rugged method is IC-ICP-MS, followed by IC-PCR-VIS. The photometric detection is subject to a minor interference in real world samples, presumably caused by carbonate. The lowest sensitivity is shown by the IC-CD method as slowest method compared, which, in addition, requires a sample pretreatment. The highest amount of information is delivered by IC-PCR-VIS, which allows the simultaneous determination of the seven standard anions and bromate.

Improved radiocarbon dating for contaminated archaeological bone collagen, silk, wool and hair samples via cross-flow nanofiltrated amino acids.

PubMed

Boudin, Mathieu; Boeckx, Pascal; Vandenabeele, Peter; Van Strydonck, Mark

2013-09-30

Radiocarbon dating and stable isotope analyses of bone collagen, wool, hair and silk contaminated with extraneous carbon (e.g. humic substances) does not yield reliable results if these materials are pre-treated using conventional methods. A cross-flow nanofiltration method was developed that can be applied to various protein materials like collagen, hair, silk, wool and leather, and should be able to remove low-molecular and high-molecular weight contaminants. To avoid extraneous carbon contamination via the filter a ceramic filter (molecular weight cut-off of 200 Da) was used. The amino acids, released by hot acid hydrolysis of the protein material, were collected in the permeate and contaminants in the retentate (>200 Da). (14)C-dating results for various contaminated archaeological samples were compared for bulk material (pre-treated with the conventional methods) and for cross-flow nanofiltrated amino acids (permeate) originating from the same samples. Contamination and quality control of (14)C dates of bulk and permeate samples were obtained by measuring C:N ratios, fluorescence spectra, and δ(13)C and δ(15)N values of the samples. Cross-flow nanofiltration decreases the C:N ratio which means that contaminants have been removed. Cross-flow nanofiltration clearly improved sample quality and (14)C results. It is a quick and non-labor-intensive technique and can easily be implemented in any (14)C and stable isotope laboratory for routine sample pre-treatment analyses. Copyright © 2013 John Wiley & Sons, Ltd.

Atmospheric corrosion of metals in industrial city environment

PubMed Central

Kusmierek, Elzbieta; Chrzescijanska, Ewa

2015-01-01

Atmospheric corrosion is a significant problem given destruction of various materials, especially metals. The corrosion investigation in the industrial city environment was carried out during one year exposure. Corrosion potential was determined using the potentiometric method. The highest effect of corrosion processes was observed during the winter season due to increased air pollution. Corrosion of samples pre-treated in tannic acid before the exposure was more difficult compared with the samples without pretreatment. The corrosion products determined with the SEM/EDS method prove that the most corrosive pollutants present in the industrial city air are SO2, CO2, chlorides and dust. PMID:26217736

Advances in paper-based sample pretreatment for point-of-care testing.

PubMed

Tang, Rui Hua; Yang, Hui; Choi, Jane Ru; Gong, Yan; Feng, Shang Sheng; Pingguan-Murphy, Belinda; Huang, Qing Sheng; Shi, Jun Ling; Mei, Qi Bing; Xu, Feng

2017-06-01

In recent years, paper-based point-of-care testing (POCT) has been widely used in medical diagnostics, food safety and environmental monitoring. However, a high-cost, time-consuming and equipment-dependent sample pretreatment technique is generally required for raw sample processing, which are impractical for low-resource and disease-endemic areas. Therefore, there is an escalating demand for a cost-effective, simple and portable pretreatment technique, to be coupled with the commonly used paper-based assay (e.g. lateral flow assay) in POCT. In this review, we focus on the importance of using paper as a platform for sample pretreatment. We firstly discuss the beneficial use of paper for sample pretreatment, including sample collection and storage, separation, extraction, and concentration. We highlight the working principle and fabrication of each sample pretreatment device, the existing challenges and the future perspectives for developing paper-based sample pretreatment technique.

Simple and Sensitive Paper-Based Device Coupling Electrochemical Sample Pretreatment and Colorimetric Detection.

PubMed

Silva, Thalita G; de Araujo, William R; Muñoz, Rodrigo A A; Richter, Eduardo M; Santana, Mário H P; Coltro, Wendell K T; Paixão, Thiago R L C

2016-05-17

We report the development of a simple, portable, low-cost, high-throughput visual colorimetric paper-based analytical device for the detection of procaine in seized cocaine samples. The interference of most common cutting agents found in cocaine samples was verified, and a novel electrochemical approach was used for sample pretreatment in order to increase the selectivity. Under the optimized experimental conditions, a linear analytical curve was obtained for procaine concentrations ranging from 5 to 60 μmol L(-1), with a detection limit of 0.9 μmol L(-1). The accuracy of the proposed method was evaluated using seized cocaine samples and an addition and recovery protocol.

Comparative AMS radiocarbon dating of pretreated versus non-pretreated tropical wood samples

NASA Astrophysics Data System (ADS)

Patrut, Adrian; von Reden, Karl F.; Lowy, Daniel A.; Mayne, Diana H.; Elder, Kathryn E.; Roberts, Mark L.; McNichol, Ann P.

2010-04-01

Several wood samples collected from Dorslandboom, a large iconic African baobab ( Adansonia digitata L.) from Namibia, were investigated by AMS radiocarbon dating subsequent to pretreatment and, alternatively, without pretreatment. The comparative statistical evaluation of results showed that there were no significant differences between fraction modern values and radiocarbon dates of the samples analyzed after pretreatment and without pretreatment, respectively. The radiocarbon date of the oldest sample was 993 ± 20 BP. Dating results also revealed that Dorslandboom is a multi-generation tree, with several stems showing different ages.

Rapid pretreatment and detection of trace aflatoxin B1 in traditional soybean sauce.

PubMed

Xie, Fang; Lai, WeiHua; Saini, Jasdeep; Shan, Shan; Cui, Xi; Liu, DaoFeng

2014-05-01

Soybean sauce, a traditional fermented food in China, has different levels of aflatoxin B1 pollution. Two kinds of direct and indirect immunomagnetic bead methods for the pretreatment of aflatoxin B1 were evaluated in this work. A method was established to detect aflatoxin B1 in soybean sauce using an immunomagnetic bead system for pretreatment and ELISA for quantification. The pretreatment method of immunomagnetic beads performed better compared with the conventional extraction and immunoaffinity column method. ELISA exhibited a good linear relationship at an aflatoxin B1 concentration of 0.05-0.3μg/kg (r(2)=0.9842). The average recoveries across spike levels varied from 0.5 to 7μg/kg were 83.6-104% with a relative standard deviation between 4.2% and 11.7%. With the advantages of rapid detection, easy operation, simple equipment, sensitivity, accuracy, and high recovery; this method can be well applied in the trace determination of aflatoxin B1 in soybean sauce samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

Influence of ultrasound pretreatment on wood physiochemical structure.

PubMed

He, Zhengbin; Wang, Zhenyu; Zhao, Zijian; Yi, Songlin; Mu, Jun; Wang, Xiaoxu

2017-01-01

As an initial step to increase the use of renewable biomass resources, this study was aimed at investigating the effects of ultrasound pretreatment on structural changes of wood. Samples were pretreated by ultrasound with the power of 300W and frequency of 28kHz in aqueous soda solution, aqueous acetic acid, or distilled water, then pretreated and control samples were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The results shown that ultrasound pretreatment is indeed effective in modifying the physiochemical structure of eucalyptus wood; the pretreatment decreased the quantity of alkali metals (e.g., potassium, calcium and magnesium) in the resulting material. Compared to the control group, the residual char content of samples pretreated in aqueous soda solution increased by 10.08%-20.12% and the reaction temperature decreased from 361°C to 341°C, however, in samples pretreated by ultrasound in acetic solution or distilled water, the residual char content decreased by 12.40%-21.45% and there were no significant differences in reactivity apart from a slightly higher maximum reaction rate. Ultrasound pretreatment increased the samples' crystallinity up to 35.5% and successfully removed cellulose, hemicellulose, and lignin from the samples; the pretreatment also increased the exposure of the sample to the treatment solutions, broke down sample pits, and generated collapses and microchannels on sample pits, and removed attachments in the samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Dispersed particle extraction--a new procedure for trace element enrichment from natural aqueous samples with subsequent ICP-OES analysis.

PubMed

Bauer, Gerald; Neouze, Marie-Alexandra; Limbeck, Andreas

2013-01-15

A novel sample pre-treatment method for multi trace element enrichment from environmental waters prior to optical emission spectrometry analysis with inductively coupled plasma (ICP-OES) is proposed, based on dispersed particle extraction (DPE). This method is based on the use of silica nanoparticles functionalized with strong cation exchange ligands. After separation from the investigated sample solution, the nanoparticles used for the extraction are directly introduced in the ICP for measurement of the adsorbed target analytes. A prerequisite for the successful application of the developed slurry approach is the use of sorbent particles with a mean size of 500 nm instead of commercially available μm sized beads. The proposed method offers the known advantages of common bead-injection (BI) techniques, and further circumvents the elution step required in conventional solid phase extraction procedures. With the use of 14.4 mL sample and addition of ammonium acetate buffer and particle slurry limits of detection (LODs) from 0.03 μg L(-1) for Be to 0.48 μg L(-1) for Fe, with relative standard deviations ranging from 1.7% for Fe and 5.5% for Cr and an average enrichment factor of 10.4 could be achieved. By implementing this method the possibility to access sorbent materials with irreversible bonding mechanisms for sample pre-treatment is established, thus improvements in the selectivity of sample pre-treatment procedures can be achieved. The presented procedure was tested for accuracy with NIST standard reference material 1643e (fresh water) and was applied to drinking water samples from the vicinity of Vienna. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid-liquid microextraction as a pretreatment method followed by high-performance liquid chromatography.

PubMed

Fan, Chen; Li, Nai; Cao, Xueli

2015-05-01

In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

Biochemical degradation and physical migration of polyphenolic compounds in osmotic dehydrated blueberries with pulsed electric field and thermal pretreatments.

PubMed

Yu, Yuanshan; Jin, Tony Z; Fan, Xuetong; Wu, Jijun

2018-01-15

Fresh blueberries were pretreated by pulsed electric fields (PEF) or thermal pretreatment and then were subject to osmotic dehydration. The changes in contents of anthocyanins, predominantly phenolic acids and flavonols, total phenolics, polyphenol oxidase (PPO) activity and antioxidant activity in the blueberry samples during pretreatment and osmotic dehydration were investigated. Biochemical degradation and physical migration of these nutritive compounds from fruits to osmotic solutions were observed during the pretreatments and osmotic dehydration. PEF pretreated samples had the least degradation loss but the most migration loss of these compounds compared to thermally pretreated and control samples. Higher rates of water loss and solid gain during osmotic dehydration were also obtained by PEF pretreatment, reducing the dehydration time from 130 to 48h. PEF pretreated and dehydrated fruits showed superior appearance to thermally pretreated and control samples. Therefore, PEF pretreatment is a preferred technology that balances nutritive quality, appearance, and dehydration rate. Published by Elsevier Ltd.

MODIFYING EPA METHOD 314.0 FOR ANALYSIS OF PERCHLORATE IN AQUEOUS SAMPLES CONTAINING HIGH TOTAL DISSOLVED SOLIDS

EPA Science Inventory

Through the Regional Applied Research Effort (RARE) program, the Chemical Exposure Research Branch and Region 9 personnel in San Francisco, California are collaborating on a project to explore sample pretreatment and preconcentration techniques to lower the method detection limit...

Cellulase digestibility of pretreated biomass is limited by cellulose accessibility.

PubMed

Jeoh, Tina; Ishizawa, Claudia I; Davis, Mark F; Himmel, Michael E; Adney, William S; Johnson, David K

2007-09-01

Attempts to correlate the physical and chemical properties of biomass to its susceptibility to enzyme digestion are often inconclusive or contradictory depending on variables such as the type of substrate, the pretreatment conditions and measurement techniques. In this study, we present a direct method for measuring the key factors governing cellulose digestibility in a biomass sample by directly probing cellulase binding and activity using a purified cellobiohydrolase (Cel7A) from Trichoderma reesei. Fluorescence-labeled T. reesei Cel7A was used to assay pretreated corn stover samples and pure cellulosic substrates to identify barriers to accessibility by this important component of cellulase preparations. The results showed cellulose conversion improved when T. reesei Cel7A bound in higher concentrations, indicating that the enzyme had greater access to the substrate. Factors such as the pretreatment severity, drying after pretreatment, and cellulose crystallinity were found to directly impact enzyme accessibility. This study provides direct evidence to support the notion that the best pretreatment schemes for rendering biomass more digestible to cellobiohydrolase enzymes are those that improve access to the cellulose in biomass cell walls, as well as those able to reduce the crystallinity of cell wall cellulose.

[Research of the surface oxide film on anodizing Ni-Cr porcelain alloy].

PubMed

Zhu, Song; Sun, Hong-Chen; Zhang, Jing-Wei; Li, Zong-Hui

2006-08-01

To study the shape, thickness and oxide percentage of major metal element of oxide film on Ni-Cr porcelain alloy after anodizing pretreatment. 10 samples were made and divided into 2 groups at random. Then after surface pretreatment, the oxide films of two samples of each group were analyzed using electronic scanning microscope. The rest 3 samples were measured by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). Lightly selective solution appeared because the different component parts of the alloy have dissimilar electrode, whose dissolve velocity were quite unlike. The sample's metal surface expanded, so the mechanical interlocking of porcelain and metal increased bond strength. The thickness of oxide film was 1.72 times of the control samples. The oxide percentage of major metal elements such as Cr, Ni and Mo were higher, especially Cr. It initially involved the formation of a thin oxide bound to the alloy and second, the ability of the formed oxide to saturate the porcelain, completing the chemical bond of porcelain to metal. The method of anodizing Ni-Cr porcelain alloy can easily control the forming of oxide film which was thin and its surface pattern was uniform. It is repeated and a good method of surface pretreatment before firing cycle.

Biodegradation of organic matters from mixed unshredded municipal solid waste through air convection before landfilling.

PubMed

Mahar, Rasool B; Liu, Jianguo; Yue, Dongbei; Nie, Yongfeng

2007-01-01

Landfilling is a dominant municipal solid waste (MSW) disposal method in most developing countries. In China, approximately 85% of the generated MSW is being disposed of in the landfills. The amount of MSW is growing rapidly with the rate of approximately 8-10% annually, which contains a high quantity of moisture and organic matters. The problems of leachate treatment and landfill gas (LFG) emissions are increasing gradually. Reducing the hazard before emplacement, pretreatment of MSW before landfilling has become very important for the conventional landfill. In this study, aerobic pretreatment of mixed MSW was used, and much attention has been given to the natural convection of air in the mixed and unshredded MSW for bioconversion of organic matter (OM). This study is an attempt to investigate aerobic pretreatment suitability for the mixed and unshredded MSW at Beijing. A pilot-scale aerobic pretreatment simulator (APS) was developed at Beishen Shu Landfill in Beijing. To work out the biodegradation of the OM in the APS, fresh and pretreated MSW samples were collected and analyzed for OM, moisture content, temperature, chemical oxygen demand, total organic carbon, carbon, nitrogen, hydrogen, lignocelluloses, and biochemical methane potential at various stages of the pretreatment. Furthermore, results of the fresh and pretreated MSW are compared. Significant reduction in the observed parameters of the pretreated waste samples is observed. This work demonstrates that pretreatment is significantly effective in reducing the landfill emissions that is leachate and LFG.

Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.

PubMed

Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann

2014-09-01

In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid LC-MS/MS quantification of the major benzodiazepines and their metabolites on dried blood spots using a simple and cost-effective sample pretreatment.

PubMed

Déglon, Julien; Versace, François; Lauer, Estelle; Widmer, Christèle; Mangin, Patrice; Thomas, Aurélien; Staub, Christian

2012-06-01

Dried blood spots (DBS) sampling has gained popularity in the bioanalytical community as an alternative to conventional plasma sampling, as it provides numerous benefits in terms of sample collection and logistics. The aim of this work was to show that these advantages can be coupled with a simple and cost-effective sample pretreatment, with subsequent rapid LC-MS/MS analysis for quantitation of 15 benzodiazepines, six metabolites and three Z-drugs. For this purpose, a simplified offline procedure was developed that consisted of letting a 5-µl DBS infuse directly into 100 µl of MeOH, in a conventional LC vial. The parameters related to the DBS pretreatment, such as extraction time or internal standard addition, were investigated and optimized, demonstrating that passive infusion in a regular LC vial was sufficient to quantitatively extract the analytes of interest. The method was validated according to international criteria in the therapeutic concentration ranges of the selected compounds. The presented strategy proved to be efficient for the rapid analysis of the selected drugs. Indeed, the offline sample preparation was reduced to a minimum, using a small amount of organic solvent and consumables, without affecting the accuracy of the method. Thus, this approach enables simple and rapid DBS analysis, even when using a non-DBS-dedicated autosampler, while lowering the costs and environmental impact.

Analysis of bromate in drinking water using liquid chromatography-tandem mass spectrometry without sample pretreatment.

PubMed

Kosaka, Koji; Asami, Mari; Takei, Kanako; Akiba, Michihiro

2011-01-01

An analytical method for determining bromate in drinking water was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The (18)O-enriched bromate was used as an internal standard. The limit of quantification (LOQ) of bromate was 0.2 µg/L. The peak of bromate was separated from those of coexisting ions (i.e., chloride, nitrate and sulfate). The relative and absolute recoveries of bromate in two drinking water samples and in a synthesized ion solution (100 mg/L chloride, 10 mg N/L nitrate, and 100 mg/L sulfate) were 99-105 and 94-105%, respectively. Bromate concentrations in 11 drinking water samples determined by LC-MS/MS were <0.2-2.3 µg/L. The results of the present study indicated that the proposed method was suitable for determining bromate concentrations in drinking water without sample pretreatment.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

PubMed

Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

2017-01-27

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Thermal/optical methods for elemental carbon quantification in soils and urban dusts: equivalence of different analysis protocols.

PubMed

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method.

Development and validation of a liquid chromatography tandem mass spectrometry assay for the quantitation of a protein therapeutic in cynomolgus monkey serum.

PubMed

Zhao, Yue; Liu, Guowen; Angeles, Aida; Hamuro, Lora L; Trouba, Kevin J; Wang, Bonnie; Pillutla, Renuka C; DeSilva, Binodh S; Arnold, Mark E; Shen, Jim X

2015-04-15

We have developed and fully validated a fast and simple LC-MS/MS assay to quantitate a therapeutic protein BMS-A in cynomolgus monkey serum. Prior to trypsin digestion, a recently reported sample pretreatment method was applied to remove more than 95% of the total serum albumin and denature the proteins in the serum sample. The pretreatment procedure simplified the biological sample prior to digestion, improved digestion efficiency and reproducibility, and did not require reduction and alkylation. The denatured proteins were then digested with trypsin at 60 °C for 30 min and the tryptic peptides were chromatographically separated on an Acquity CSH column (2.1 mm × 50 mm, 1.7 μm) using gradient elution. One surrogate peptide was used for quantitation and another surrogate peptide was selected for confirmation. Two corresponding stable isotope labeled peptides were used to compensate variations during LC-MS detection. The linear analytical range of the assay was 0.50-500 μg/mL. The accuracy (%Dev) was within ± 5.4% and the total assay variation (%CV) was less than 12.0% for sample analysis. The validated method demonstrated good accuracy and precision and the application of the innovative albumin removal sample pretreatment method improved both assay sensitivity and robustness. The assay has been applied to a cynomolgus monkey toxicology study and the serum sample concentration data were in good agreement with data generated using a quantitative ligand-binding assay (LBA). The use of a confirmatory peptide, in addition to the quantitation peptide, ensured the integrity of the drug concentrations measured by the method. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of species, pretreatments, and drying methods on the functional and pasting properties of high-quality yam flour.

PubMed

Wahab, Bashirat A; Adebowale, Abdul-Rasaq A; Sanni, Silifat A; Sobukola, Olajide P; Obadina, Adewale O; Kajihausa, Olatundun E; Adegunwa, Mojisola O; Sanni, Lateef O; Tomlins, Keith

2016-01-01

The study investigated the functional properties of HQYF (high-quality yam flour) from tubers of four dioscorea species. The tubers were processed into HQYF using two pretreatments (potassium metabisulphite: 0.28%, 15 min; blanching: 70°C, 15 min) and drying methods (cabinet: 60°C, 48 h; sun drying: 3 days). Significant differences (P < 0.05) were observed in pasting characteristics of flours among the four species. The drying method significantly affected only the peak viscosity. The interactive effect of species, pretreatment, and drying methods on the functional properties was significant (P < 0.05) except for emulsification capacity, angle of repose, and least gelation concentration. The significant variation observed in most of the functional properties of the HQYF could contribute significantly to breeding programs of the yam species for diverse food applications. The pastes of flour from Dioscorea dumetorum pretreated with potassium metabisulphite and dried under a cabinet dryer were stable compared to other samples, hence will have better applications in products requiring lower retrogradation during freeze/thaw cycles.

Effect of biological pretreatments in enhancing corn straw biogas production.

PubMed

Zhong, Weizhang; Zhang, Zhongzhi; Luo, Yijing; Sun, Shanshan; Qiao, Wei; Xiao, Meng

2011-12-01

A biological pretreatment with new complex microbial agents was used to pretreat corn straw at ambient temperature (about 20°C) to improve its biodegradability and anaerobic biogas production. A complex microbial agent dose of 0.01% (w/w) and pretreatment time of 15 days were appropriate for biological pretreatment. These treatment conditions resulted in 33.07% more total biogas yield, 75.57% more methane yield, and 34.6% shorter technical digestion time compared with the untreated sample. Analyses of chemical compositions showed 5.81-25.10% reductions in total lignin, cellulose, and hemicellulose contents, and 27.19-80.71% increases in hot-water extractives; these changes contributed to the enhancement of biogas production. Biological pretreatment could be an effective method for improving biodegradability and enhancing the highly efficient biological conversion of corn straw into bioenergy. Copyright © 2011 Elsevier Ltd. All rights reserved.

A highly sensitive and specific method for the screening detection of genetically modified organisms based on digital PCR without pretreatment

PubMed Central

Fu, Wei; Zhu, Pengyu; Wang, Chenguang; Huang, Kunlun; Du, Zhixin; Tian, Wenying; Wang, Qin; Wang, Huiyu; Xu, Wentao; Zhu, Shuifang

2015-01-01

Digital PCR has developed rapidly since it was first reported in the 1990s. It was recently reported that an improved method facilitated the detection of genetically modified organisms (GMOs). However, to use this improved method, the samples must be pretreated, which could introduce inaccuracy into the results. In our study, we explored a pretreatment-free digital PCR detection method for the screening for GMOs. We chose the CaMV35s promoter and the NOS terminator as the templates in our assay. To determine the specificity of our method, 9 events of GMOs were collected, including MON810, MON863, TC1507, MIR604, MIR162, GA21, T25, NK603 and Bt176. Moreover, the sensitivity, intra-laboratory and inter-laboratory reproducibility of our detection method were assessed. The results showed that the limit of detection of our method was 0.1%, which was lower than the labeling threshold level of the EU. The specificity and stability among the 9 events were consistent, respectively. The intra-laboratory and inter-laboratory reproducibility were both good. Finally, the perfect fitness for the detection of eight double-blind samples indicated the good practicability of our method. In conclusion, the method in our study would allow more sensitive, specific and stable screening detection of the GMO content of international trading products. PMID:26239916

A highly sensitive and specific method for the screening detection of genetically modified organisms based on digital PCR without pretreatment.

PubMed

Fu, Wei; Zhu, Pengyu; Wang, Chenguang; Huang, Kunlun; Du, Zhixin; Tian, Wenying; Wang, Qin; Wang, Huiyu; Xu, Wentao; Zhu, Shuifang

2015-08-04

Digital PCR has developed rapidly since it was first reported in the 1990 s. It was recently reported that an improved method facilitated the detection of genetically modified organisms (GMOs). However, to use this improved method, the samples must be pretreated, which could introduce inaccuracy into the results. In our study, we explored a pretreatment-free digital PCR detection method for the screening for GMOs. We chose the CaMV35s promoter and the NOS terminator as the templates in our assay. To determine the specificity of our method, 9 events of GMOs were collected, including MON810, MON863, TC1507, MIR604, MIR162, GA21, T25, NK603 and Bt176. Moreover, the sensitivity, intra-laboratory and inter-laboratory reproducibility of our detection method were assessed. The results showed that the limit of detection of our method was 0.1%, which was lower than the labeling threshold level of the EU. The specificity and stability among the 9 events were consistent, respectively. The intra-laboratory and inter-laboratory reproducibility were both good. Finally, the perfect fitness for the detection of eight double-blind samples indicated the good practicability of our method. In conclusion, the method in our study would allow more sensitive, specific and stable screening detection of the GMO content of international trading products.

Towards a method of rapid extraction of strontium-90 from urine: urine pretreatment and alkali metal removal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hawkins, C.; Dietz, M.; Kaminski, M.

2016-03-01

A technical program to support the Centers of Disease Control and Prevention is being developed to provide an analytical method for rapid extraction of Sr-90 from urine, with the intent of assessing the general population’s exposure during an emergency response to a radiological terrorist event. Results are presented on the progress in urine sample preparation and chemical separation steps that provide an accurate and quantitative detection of Sr-90 based upon an automated column separation sequence and a liquid scintillation assay. Batch extractions were used to evaluate the urine pretreatment and the column separation efficiency and loading capacity based upon commercial,more » extractant-loaded resins. An efficient pretreatment process for decolorizing and removing organics from urine without measurable loss of radiostrontium from the sample was demonstrated. In addition, the Diphonix® resin shows promise for the removal of high concentrations of common strontium interferents in urine as a first separation step for Sr-90 analysis.« less

A laboratory-scale pretreatment and hydrolysis assay for determination of reactivity in cellulosic biomass feedstocks.

PubMed

Wolfrum, Edward J; Ness, Ryan M; Nagle, Nicholas J; Peterson, Darren J; Scarlata, Christopher J

2013-11-14

The rapid determination of the release of structural sugars from biomass feedstocks is an important enabling technology for the development of cellulosic biofuels. An assay that is used to determine sugar release for large numbers of samples must be robust, rapid, and easy to perform, and must use modest amounts of the samples to be tested.In this work we present a laboratory-scale combined pretreatment and saccharification assay that can be used as a biomass feedstock screening tool. The assay uses a commercially available automated solvent extraction system for pretreatment followed by a small-scale enzymatic hydrolysis step. The assay allows multiple samples to be screened simultaneously, and uses only ~3 g of biomass per sample. If the composition of the biomass sample is known, the results of the assay can be expressed as reactivity (fraction of structural carbohydrate present in the biomass sample released as monomeric sugars). We first present pretreatment and enzymatic hydrolysis experiments on a set of representative biomass feedstock samples (corn stover, poplar, sorghum, switchgrass) in order to put the assay in context, and then show the results of the assay applied to approximately 150 different feedstock samples covering 5 different materials. From the compositional analysis data we identify a positive correlation between lignin and structural carbohydrates, and from the reactivity data we identify a negative correlation between both carbohydrate and lignin content and total reactivity. The negative correlation between lignin content and total reactivity suggests that lignin may interfere with sugar release, or that more mature samples (with higher structural sugars) may have more recalcitrant lignin. The assay presented in this work provides a robust and straightforward method to measure the sugar release after pretreatment and saccharification that can be used as a biomass feedstock screening tool. We demonstrated the utility of the assay by identifying correlations between feedstock composition and reactivity in a population of 150 samples.

Evaluation of Mediterranean Agricultural Residues as a Potential Feedstock for the Production of Biogas via Anaerobic Fermentation.

PubMed

Nitsos, Christos; Matsakas, Leonidas; Triantafyllidis, Kostas; Rova, Ulrika; Christakopoulos, Paul

2015-01-01

Hydrothermal, dilute acid, and steam explosion pretreatment methods, were evaluated for their efficiency to improve the methane production yield of three Mediterranean agricultural lignocellulosic residues such as olive tree pruning, grapevine pruning, and almond shells. Hydrothermal and dilute acid pretreatments provided low to moderate increase in the digestibility of the biomass samples, whereas steam explosion enabled the highest methane yields to be achieved for almond shells at 232.2 ± 13.0 mL CH4/gVS and olive pruning at 315.4 ± 0.0 mL CH4/gVS. Introduction of an enzymatic prehydrolysis step moderately improved methane yields for hydrothermal and dilute acid pretreated samples but not for the steam exploded ones.

Evaluation of Mediterranean Agricultural Residues as a Potential Feedstock for the Production of Biogas via Anaerobic Fermentation

PubMed Central

Nitsos, Christos; Triantafyllidis, Kostas

2015-01-01

Hydrothermal, dilute acid, and steam explosion pretreatment methods, were evaluated for their efficiency to improve the methane production yield of three Mediterranean agricultural lignocellulosic residues such as olive tree pruning, grapevine pruning, and almond shells. Hydrothermal and dilute acid pretreatments provided low to moderate increase in the digestibility of the biomass samples, whereas steam explosion enabled the highest methane yields to be achieved for almond shells at 232.2 ± 13.0 mL CH4/gVS and olive pruning at 315.4 ± 0.0 mL CH4/gVS. Introduction of an enzymatic prehydrolysis step moderately improved methane yields for hydrothermal and dilute acid pretreated samples but not for the steam exploded ones. PMID:26609521

Bioethanol production from rice husk using different pretreatments and fermentation conditions.

PubMed

Madu, Joshua Osuigwe; Agboola, Bolade Oyeyinka

2018-01-01

Bioethanol is an environmentally friendly alternative to petroleum energy sources. This study evaluated the effects of H 2 O, HCl, NaOH and FeCl 3 pretreated rice husk feedstocks on the production of bioethanol. The pretreatments were carried out using water, 0.1 M HCl, NaOH and FeCl 3 at 121 °C for 15 min, followed by simultaneous saccharification and fermentation (SSF) as well as separate hydrolysis and fermentation (SHF). The raw and pretreated lignocellulosic feedstocks were analyzed using Fourier transform infrared spectroscopy. Saccharification and fermentation were accomplished using Trichoderma reesei cellulase and Saccharomyces cerevisiae , respectively. The products obtained after saccharification and fermentation were collected and analyzed for reducing sugars and ethanol contents using 3,5-dinitrosalicylic acid and high-performance liquid chromatography, respectively. Enzyme hydrolysis of the FeCl 3 and HCl treated samples resulted in hydrolysates containing 3.845 and 3.402 mg/ml glucose equivalent, respectively. In all pretreatments, SSF for each pretreatment produced more ethanol than the SHF method; the FeCl 3 pretreatment gave the highest ethanol yield of 3.011 ± 0.034 and 3.802 ± 0.041% in the SHF and SSF methods, respectively. Utilization of FeCl 3 pretreatment of rice husk is a potential option for bioethanol production in the future.

A process to preserve valuable compounds and acquire essential oils from pomelo flavedo using a microwave irradiation treatment.

PubMed

Liu, Zaizhi; Zu, Yuangang; Yang, Lei

2017-06-01

A microwave pretreatment method was developed to preserve pectin, naringin, and limonin contents in pomelo flavedo to allow for longer storage times and subsequent extraction of pomelo essential oil. In terms of the essential oil, microwave pretreatment performed better than hydrodistillation with respect to extraction efficiency (1.88±0.06% in 24min versus 1.91±0.08% in 240min), oxygenation fraction (48.59±1.32% versus 29.63±1.02%), energy consumption (0.15kWh versus 1.54kWh), and environmental impact (123.20g CO 2 versus 1232g CO 2 ). Microwave-pretreated samples retained higher amounts of pectin, naringin, and limonin compared with non-pretreated samples. No obvious change in the degree of pectin esterification was observed. This study shows that the proposed process is a promising methodology for both preserving valuable compounds in pomelo flavedo during storage and acquiring essential oils. Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterization of Nanofibrillated Cellulose Produced by Different Methods from Cabbage Outer Leaves.

PubMed

Khukutapan, Donnapa; Chiewchan, Naphaporn; Devahastin, Sakamon

2018-06-01

The potential use of cabbage outer leaves as a starting material for the production of nanofibrillated cellulose (NFC) was investigated. Chemical-free pretreatment methods, namely, autoclaving, ultrasonication (US), and high-shear homogenization (HS), were applied to remove noncellulosic components from cabbage cell walls prior to defibrillation, which was conducted by subjecting a pretreated sample to HS and then high-pressure homogenization. The sample undergone autoclaving at 130 °C for 2 hr was noted to contain a significantly higher cellulose content (36.5% dry mass) compared with the fresh leaves (12.48% dry mass). This led to an increase in the crystallinity index (CI) of the autoclaved cabbages from 30.8% to 50.7%. Further increase in the cellulose content (47.0% to 49.2% dry mass) was observed when subjecting the autoclaved sample to either US at 37 kHz for 1 hr, HS at 3800 × g for 15 min or HS followed by US at the aforementioned conditions. After pretreatment and defibrilllation, a suspension of NFC with the diameters of 4 to 50 nm was obtained, with the CI of 59.1% to 66.7%. Such a suspension exhibited a gel-like behavior with tan δ in the range of 0.12 to 0.13; the suspension exhibited a similar behavior to that prepared by the conventional chemical pretreatment method. NFC could be produced from cabbage outer leaves, which are an abundantly available by-product of a vegetable processing plant, via the combined hydrothermal and mechanical pretreatment without the use of any chemicals. This chemical-free preparation process is highly desirable as it leaves no residues in the product and causes no chemical waste that needs to be treated. Cabbage-based NFC also exhibits similar characteristics to that prepared via a chemically treated route. © 2018 Institute of Food Technologists®.

Role of modifier in microwave assisted extraction of oleanolic acid from Gymnema sylvestre: application of green extraction technology for botanicals.

PubMed

Mandal, Vivekananda; Dewanjee, Saikat; Mandal, Subhash C

2009-08-01

This work highlights the development of a green extraction technology for botanicals with the use of microwave energy. Taking into consideration the extensive time involved in conventional extraction methods, coupled with usage of large volumes of organic solvent and energy resources, an ecofriendly green method that can overcome the above problems has been developed. The work compares the effect of sample pretreatment with untreated sample for improved yield of oleanolic acid from Gymnema sylvestre leaves. The pretreated sample with water produced 0.71% w/w oleanolic acid in one extraction cycle with 500 W microwave power, 25 mL methanol and only an 8 min extraction time. On the other hand, a conventional heat reflux extraction for 6 hours could produce only 0.62% w/w oleanolic acid. The detailed mechanism of extraction has been studied through scanning electron micrographs. The environmental impact of the proposed green method has also been evaluated.

Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

PubMed

Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

2015-05-01

A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (<10%) for phenols. Four real soil samples were analyzed by the proposed method to assess its applicability. Experimental results showed that the soil samples were free of our target compounds, and average recoveries were in the range of 87.9-110%. These findings indicate that accelerated solvent extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

PubMed

Lin, Li; Chen, Guang; Chen, Yuhong

2011-07-01

A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

Quantification of acidic compounds in complex biomass-derived streams

DOE PAGES

Karp, Eric M.; Nimlos, Claire T.; Deutch, Steve; ...

2016-05-10

Biomass-derived streams that contain acidic compounds from the degradation of lignin and polysaccharides (e.g. black liquor, pyrolysis oil, pyrolytic lignin, etc.) are chemically complex solutions prone to instability and degradation during analysis, making quantification of compounds within them challenging. Here we present a robust analytical method to quantify acidic compounds in complex biomass-derived mixtures using ion exchange, sample reconstitution in pyridine and derivatization with BSTFA. The procedure is based on an earlier method originally reported for kraft black liquors and, in this work, is applied to identify and quantify a large slate of acidic compounds in corn stover derived alkalinemore » pretreatment liquor (APL) as a function of pretreatment severity. Analysis of the samples is conducted with GCxGC-TOFMS to achieve good resolution of the components within the complex mixture. The results reveal the dominant low molecular weight components and their concentrations as a function of pretreatment severity. Application of this method is also demonstrated in the context of lignin conversion technologies by applying it to track the microbial conversion of an APL substrate. Here as well excellent results are achieved, and the appearance and disappearance of compounds is observed in agreement with the known metabolic pathways of two bacteria, indicating the sample integrity was maintained throughout analysis. Finally, it is shown that this method applies more generally to lignin-rich materials by demonstrating its usefulness in analysis of pyrolysis oil and pyrolytic lignin.« less

Investigation of Pleurotus ostreatus pretreatment on switchgrass for ethanol production

NASA Astrophysics Data System (ADS)

Slavens, Shelyn Gehle

Fungal pretreatment using the white-rot fungus Pleurotus ostreatus on switchgrass for ethanol production was studied. In a small-scale storage study, small switchgrass bales were inoculated with fungal spawn and automatically watered to maintain moisture. Sampled at 25, 53, and 81 d, the switchgrass composition was determined and liquid hot water (LHW) pretreatment was conducted. Fungal pretreatment significantly decreased the xylan and lignin content; glucan was not significantly affected by fungal loading. The glucan, xylan, and lignin contents significantly decreased with increased fungal pretreatment time. The effects of the fungal pretreatment were not highly evident after the LHW pretreatment, showing only changes based on sampling time. Although other biological activity within the bales increased cellulose degradation, the fungal pretreatment successfully reduced the switchgrass lignin and hemicellulose contents. In a laboratory-scale nutrient supplementation study, copper, manganese, glucose, or water was added to switchgrass to induce production of ligninolytic enzymes by P. ostreatus. After 40 d, ligninolytic enzyme activities and biomass composition were determined and simultaneous saccharification and fermentation (SSF) was conducted to determine ethanol yield. Laccase activity was similar for all supplements and manganese peroxidase (MnP) activity was significantly less in copper-treated samples than in the other fungal-inoculated samples. The fungal pretreatment reduced glucan, xylan, and lignin content, while increasing extractable sugars content. The lowest lignin contents occurred in the water-fungal treated samples and produced the greatest ethanol yields. The greatest lignin contents occurred in the copper-fungal treated samples and produced the lowest ethanol yields. Manganese-fungal and glucose-fungal treated samples had similar, intermediate lignin contents and produced similar, intermediate ethanol yields. Ethanol yields from switchgrass were increased significantly by fungal pretreatment.

Color and alcohol removal for the simultaneous detection of amino acids and sugars in wine by two-dimensional ion chromatography.

PubMed

Fa, Yun; Liu, Yinghui; Xu, Aihua; Yu, Yuexue; Li, Fangfang; Liu, Huizhou

2017-09-15

An effective pretreatment method for wine color removal by a PS-DVB SPE cartridge and online alcohol elimination by valve switching was presented. The optimum parameters for color removal were investigated: 40-μm and 100Å poly (styrene)-divinylbenzene (PS-DVB) (0.4g) was selected as the color removal material and 5mL of ethanol (10%) as the elution solvent for sample pretreatment under given condition. Moreover, an accurate and automated two-dimensional ion chromatography method for the simultaneous detection of amino acids and sugars was achieved with two valves after injection without alcohol interference. The method had a mean correlation coefficient of >0.99 and a repeatability of 0.92%-4.30% for eight replicates. The mean recovery of six red wine samples were 97.6%, 96.6%, 96.1%, 95.9%, 97.3% and 96.4% respectively. And this method successfully analyzed the amino acid and sugar contents of six wine samples of different origins. Copyright © 2017. Published by Elsevier B.V.

A porphyrin-based fluorescence method for zinc determination in commercial propolis extracts without sample pretreatment.

PubMed

Pierini, Gastón Darío; Pinto, Victor Hugo A; Maia, Clarissa G C; Fragoso, Wallace D; Reboucas, Julio S; Centurión, María Eugenia; Pistonesi, Marcelo Fabián; Di Nezio, María Susana

2017-11-01

The quantification of zinc in over-the-counter drugs as commercial propolis extracts by molecular fluorescence technique using meso-tetrakis(4-carboxyphenyl)porphyrin (H 2 TCPP 4 ) was developed for the first time. The calibration curve is linear from 6.60 to 100 nmol L -1 of Zn 2+ . The detection and quantification limits were 6.22 nmol L -1 and 19.0 nmol L -1 , respectively. The reproducibility and repeatability calculated as the percentage variation of slopes of seven calibration curves were 6.75% and 4.61%, respectively. Commercial propolis extract samples from four Brazilian states were analyzed and the results (0.329-0.797 mg/100 mL) obtained with this method are in good agreement with that obtained with the Atomic Absorption Spectroscopy (AAS) technique. The method is simple, fast, of low cost and allows the analysis of the samples without pretreatment. Moreover the major advantage is that Zn-porphyrin complex presents fluorescent characteristic promoting the selectivity and sensitivity of the method. Copyright © 2017 John Wiley & Sons, Ltd.

Influence of Adhesives and Methods of Enamel Pretreatment on the Shear Bond Strength of Orthodontic Brackets

PubMed Central

Jurišić, Sanja; Jurišić, Gordan

2015-01-01

Aim The objective of present study was to examine influence of adhesives and methods of enamel pretreatment on the shear bond strength (SBS) of orthodontic brackets. The adhesives used were resin-reinforced glass ionomer cements-GIC (Fuji Ortho LC) and composite resin (Transbond XT). Material and Methods The experimental sample consisted of 80 extracted human first premolars. The sample was divided into four equal groups, and the metal brackets were bonded with different enamel pretreatments by using two adhesives: group A-10% polyacrylic acid; Fuji Ortho LC, group B–37% phosphoric acid; Fuji Ortho LC, group C–self etching primer; Transbond XT, group D–37% phosphoric acid, primer; Transbond XT. SBS of brackets was measured. After debonding of brackets, the adhesive remnant index (ARI) was evaluated. Results After the statistical analysis of the collected data was performed (ANOVA; Sheffe post-hoc test), the results showed that significantly lower SBS of the group B was found in relation to the groups C (p=0.031) and D (p=0.026). The results of ARI were similar in all testing groups and it was not possible to determine any statistically significant difference of the ARI (Chi- square test) between all four experimental groups. Conclusion The conclusion is that the use of composite resins material with appropriate enamel pretreatment according to manufacturer’s recommendation is the “gold standard” for brackets bonding for fixed orthodontic appliances. PMID:27688410

Development and validation of a simplified titration method for monitoring volatile fatty acids in anaerobic digestion.

PubMed

Sun, Hao; Guo, Jianbin; Wu, Shubiao; Liu, Fang; Dong, Renjie

2017-09-01

The volatile fatty acids (VFAs) concentration has been considered as one of the most sensitive process performance indicators in anaerobic digestion (AD) process. However, the accurate determination of VFAs concentration in AD processes normally requires advanced equipment and complex pretreatment procedures. A simplified method with fewer sample pretreatment procedures and improved accuracy is greatly needed, particularly for on-site application. This report outlines improvements to the Nordmann method, one of the most popular titrations used for VFA monitoring. The influence of ion and solid interfering subsystems in titrated samples on results accuracy was discussed. The total solid content in titrated samples was the main factor affecting accuracy in VFA monitoring. Moreover, a high linear correlation was established between the total solids contents and VFA measurement differences between the traditional Nordmann equation and gas chromatography (GC). Accordingly, a simplified titration method was developed and validated using a semi-continuous experiment of chicken manure anaerobic digestion with various organic loading rates. The good fitting of the results obtained by this method in comparison with GC results strongly supported the potential application of this method to VFA monitoring. Copyright © 2017. Published by Elsevier Ltd.

Effect of EDTA Conditioning and Carbodiimide Pretreatment on the Bonding Performance of All-in-One Self-Etch Adhesives

PubMed Central

Singh, Shipra; Nagpal, Rajni; Tyagi, Shashi Prabha; Manuja, Naveen

2015-01-01

Objective. This study evaluated the effect of ethylenediaminetetraacetic acid (EDTA) conditioning and carbodiimide (EDC) pretreatment on the shear bond strength of two all-in-one self-etch adhesives to dentin. Methods. Flat coronal dentin surfaces were prepared on one hundred and sixty extracted human molars. Teeth were randomly divided into eight groups according to two different self-etch adhesives used [G-Bond and OptiBond-All-In-One] and four different surface pretreatments: (a) adhesive applied following manufacturer's instructions; (b) dentin conditioning with 24% EDTA gel prior to application of adhesive; (c) EDC pretreatment followed by application of adhesive; (d) application of EDC on EDTA conditioned dentin surface followed by application of adhesive. Composite restorations were placed in all the samples. Ten samples from each group were subjected to immediate and delayed (6-month storage in artificial saliva) shear bond strength evaluation. Data collected was subjected to statistical analysis using three-way ANOVA and post hoc Tukey's test at a significance level of p < 0.05.  Results and Conclusion. EDTA preconditioning as well as EDC pretreatment alone had no significant effect on the immediate and delayed bond strengths of either of the adhesives. However, EDC pretreatment on EDTA conditioned dentin surface resulted in preservation of resin-dentin bond strength of both adhesives with no significant fall over six months. PMID:26557850

Specific pretreatments reduce curing period of vanilla (Vanilla planifolia) beans.

PubMed

Sreedhar, R V; Roohie, K; Venkatachalam, L; Narayan, M S; Bhagyalakshmi, N

2007-04-18

With the aiming of reducing the curing period, effects of pretreatments on flavor formation in vanilla beans during accelerated curing at 38 degrees C for 40 days were studied. Moisture loss, change in texture, levels of flavoring compounds, and activities of relevant enzymes were compared among various pretreatments as well as the commercial sample. Use of naphthalene acetic acid (NAA; 5 mg/L) or Ethrel (1%) with blanching pretreatment resulted in 3-fold higher vanillin on the 10th day. Other flavoring compounds-vanillic acid, p-hydroxybenzoic acid, and p-hydroxybenzaldehyde-fluctuated greatly, showing no correlation with the pretreatments. Scarification of beans resulted in nearly 4- and 3.6-fold higher vanillin formations on the 10th day in NAA- and Ethrel-treated beans, respectively, as compared to control with a significant change in texture. When activities of major relevant enzymes were followed, addition of NAA or Ethrel helped to retain higher levels of cellulase throughout the curing period and higher levels of beta-glucosidase on the 20th day that correlated with higher vanillin content during curing and subsequent periods. Peroxidase, being highest throughout, did not correlate with the change in levels of major flavoring compounds. The pretreatment methods of the present study may find importance for realizing higher flavor formation in a shorter period because the major quality parameters were found to be comparable to those of a commercial sample.

Treatment of olive mill wastewater by chemical processes: effect of acid cracking pretreatment.

PubMed

Hande Gursoy-Haksevenler, B; Arslan-Alaton, Idil

2014-01-01

The effect of acid cracking (pH 2.0; T 70 °C) and filtration as a pretreatment step on the chemical treatability of olive mill wastewater (chemical oxygen demand (COD) 150,000 m/L; total organic carbon (TOC) 36,000 mg/L; oil-grease 8,200 mg/L; total phenols 3,800 mg/L) was investigated. FeCl3 coagulation, Ca(OH)2 precipitation, electrocoagulation using stainless steel electrodes and the Fenton's reagent were applied as chemical treatment methods. Removal performances were examined in terms of COD, TOC, oil-grease, total phenols, colour, suspended solids and acute toxicity with the photobacterium Vibrio fischeri. Significant oil-grease (95%) and suspended solids (96%) accompanied with 58% COD, 43% TOC, 39% total phenols and 80% colour removals were obtained by acid cracking-filtration pretreatment. Among the investigated chemical treatment processes, electrocoagulation and the Fenton's reagent were found more effective after pretreatment, especially in terms of total phenols removal. Total phenols removal increased from 39 to 72% when pretreatment was applied, while no significant additional (≈10-15%) COD and TOC removals were obtained when acid cracking was coupled with chemical treatment. The acute toxicity of the original olive mill wastewater sample increased considerably after pretreatment from 75 to 89% (measured for the 10-fold diluted wastewater sample). An operating cost analysis was also performed for the selected chemical treatment processes.

The effect of dilute acid pre-treatment process in bioethanol production from durian (Durio zibethinus) seeds waste

NASA Astrophysics Data System (ADS)

Ghazali, K. A.; Salleh, S. F.; Riayatsyah, T. M. I.; Aditiya, H. B.; Mahlia, T. M. I.

2016-03-01

Lignocellulosic biomass is one of the promising feedstocks for bioethanol production. The process starts from pre-treatment, hydrolysis, fermentation, distillation and finally obtaining the final product, ethanol. The efficiency of enzymatic hydrolysis of cellulosic biomass depends heavily on the effectiveness of the pre-treatment step which main function is to break the lignin structure of the biomass. This work aims to investigate the effects of dilute acid pre-treatment on the enzymatic hydrolysis of durian seeds waste to glucose and the subsequent bioethanol fermentation process. The yield of glucose from dilute acid pre-treated sample using 0.6% H2SO4 and 5% substrate concentration shows significant value of 23.4951 g/L. Combination of dilute acid pre-treatment and enzymatic hydrolysis using 150U of enzyme able to yield 50.0944 g/L of glucose content higher compared to normal pre-treated sample of 8.1093 g/L. Dilute acid pre-treatment sample also shows stable and efficient yeast activity during fermentation process with lowest glucose content at 2.9636 g/L compared to 14.7583g/L for normal pre-treated sample. Based on the result, it can be concluded that dilute acid pre-treatment increase the yield of ethanol from bioethanol production process.

Development of an improved rapid BACpro® protocol and a method for direct identification from blood-culture-positive bottles using matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

PubMed

Yonezawa, Takatoshi; Watari, Tomohisa; Ashizawa, Kazuho; Hanada, Daisuke; Yanagiya, Takako; Watanabe, Naoki; Terada, Takashi; Tomoda, Yutaka; Fujii, Satoshi

2018-05-01

Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been incorporated into pathogenic bacterial identification methods and has improved their rapidity. Various methods have been reported to directly identify bacteria with MALDI-TOF MS by pretreating culture medium in blood culture bottles. Rapid BACpro® (Nittobo Medical Co., Ltd.) is a pretreatment kit for effective collection of bacteria with cationic copolymers. However, the Rapid BACpro® pretreatment kit is adapted only for MALDI Biotyper (Bruker Daltonics K.K.), and there has been a desire to expand its use to VITEK MS (VMS; bioMerieux SA). We improved the protocol and made it possible to analyze with VMS. The culture medium bacteria collection method was changed to a method with centrifugation after hemolysis using saponin; the cationic copolymer concentration was changed to 30% of the original concentration; the sequence with which reagents were added was changed; and a change was made to an ethanol/formic acid extraction method. The improved protocol enhanced the identification performance. When VMS was used, the identification rate was 100% with control samples. With clinical samples, the identification agreement rate with the cell smear method was 96.3%. The improved protocol is effective in blood culture rapid identification, being both simpler and having an improved identification performance compared with the original. Copyright © 2018 Elsevier B.V. All rights reserved.

Thermal/Optical Methods for Elemental Carbon Quantification in Soils and Urban Dusts: Equivalence of Different Analysis Protocols

PubMed Central

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method. PMID:24358286

Enhanced biomass delignification and enzymatic saccharification of canola straw by steam-explosion pretreatment.

PubMed

Garmakhany, Amir Daraei; Kashaninejad, Mahdi; Aalami, Mehran; Maghsoudlou, Yahya; Khomieri, Mortza; Tabil, Lope G

2014-06-01

In recent decades, bioconversion of lignocellulosic biomass to biofuel (ethanol and biodiesel) has been extensively investigated. The three main chemical constituents of biomass are cellulose, hemicellulose and lignin. Cellulose and hemicellulose are polysaccharides of primarily fermentable sugars, glucose and xylose respectively. Hemicellulose also includes small fermentable fractions of arabinose, galactose and mannose. The main issue in converting lignocellulosic biomass to fuel ethanol is the accessibility of the polysaccharides for enzymatic breakdown into monosaccharides. This study focused on the use of steam explosion as the pretreatment method for canola straw as lignocellulosic biomass. Result showed that steam explosion treatment of biomass increased cellulose accessibility and it hydrolysis by enzyme hydrolysis. Following 72 h of enzyme hydrolysis, a maximum cellulose conversion to glucose yield of 29.40% was obtained for the steam-exploded sample while the control showed 11.60% glucose yields. Steam explosion pretreatment increased glucose production and glucose yield by 200% and 153.22%, respectively, compared to the control sample. The crystalline index increased from 57.48% in untreated canola straw to 64.72% in steam-exploded samples. Steam explosion pretreatment of biomass increased cellulose accessibility, and enzymatic hydrolysis increased glucose production and glucose yield of canola straw. © 2013 Society of Chemical Industry.

Rapid fingerprinting and classification of extra virgin olive oil by microjet sampling and extractive electrospray ionization mass spectrometry.

PubMed

Law, Wai Siang; Chen, Huan Wen; Balabin, Roman; Berchtold, Christian; Meier, Lukas; Zenobi, Renato

2010-04-01

Microjet sampling in combination with extractive electrospray ionization (EESI) mass spectrometry (MS) was applied to the rapid characterization and classification of extra virgin olive oil (EVOO) without any sample pretreatment. When modifying the composition of the primary ESI spray solvent, mass spectra of an identical EVOO sample showed differences. This demonstrates the capability of this technique to extract molecules with varying polarities, hence generating rich molecular information of the EVOO. Moreover, with the aid of microjet sampling, compounds of different volatilities (e.g.E-2-hexenal, trans-trans-2,4-heptadienal, tyrosol and caffeic acid) could be sampled simultaneously. EVOO data was also compared with that of other edible oils. Principal Component Analysis (PCA) was performed to discriminate EVOO and EVOO adulterated with edible oils. Microjet sampling EESI-MS was found to be a simple, rapid (less than 2 min analysis time per sample) and powerful method to obtain MS fingerprints of EVOO without requiring any complicated sample pretreatment steps.

A rapid HPLC column switching method for sample preparation and determination of β-carotene in food supplements.

PubMed

Brabcová, Ivana; Hlaváčková, Markéta; Satínský, Dalibor; Solich, Petr

2013-11-15

A simple and automated HPLC column-switching method with rapid sample pretreatment has been developed for quantitative determination of β-carotene in food supplements. Commercially samples of food supplements were dissolved in chloroform with help of saponification with 1M solution of sodium hydroxide in ultrasound bath. A 20-min sample dissolution/extraction step was necessary before chromatography analysis to transfer β-carotene from solid state of food supplements preparations (capsules,tablets) to chloroform solution. Sample volume - 3μL of chloroform phase was directly injected into the HPLC system. Next on-line sample clean-up was achieved on the pretreatment precolumn Chromolith Guard Cartridge RP-18e (Merck), 10×4.6mm, with a washing mobile phase (methanol:water, 92:8, (v/v)) at a flow rate of 1.5mL/min. Valve switch to analytical column was set at 2.5min in a back-flush mode. After column switching to the analytical column Ascentis Express C-18, 30×4.6mm, particle size 2.7μm (Sigma Aldrich), the separation and determination of β-carotene in food supplements was performed using a mobile phase consisting of 100% methanol, column temperature at 60°C and flow rate 1.5mL/min. The detector was set at 450nm. Under the optimum chromatographic conditions standard calibration curve was measured with good linearity - correlation coefficient for β-carotene (r(2)=0.999014; n=6) between the peak areas and concentration of β-carotene 20-200μg/mL. Accuracy of the method defined as a mean recovery was in the range 96.66-102.40%. The intraday method precision was satisfactory at three concentration levels 20, 125 and 200μg/mL and relative standard deviations were in the range 0.90-1.02%. The chromatography method has shown high sample throughput during column-switching pretreatment process and analysis in one step in short time (6min) of the whole chromatographic analysis. Copyright © 2013 Elsevier Ltd. All rights reserved.

Influence of Adhesives and Methods of Enamel Pretreatment on the Shear Bond Strength of Orthodontic Brackets.

PubMed

Jurišić, Sanja; Jurišić, Gordan; Jurić, Hrvoje

2015-12-01

The objective of present study was to examine influence of adhesives and methods of enamel pretreatment on the shear bond strength (SBS) of orthodontic brackets. The adhesives used were resin-reinforced glass ionomer cements-GIC (Fuji Ortho LC) and composite resin (Transbond XT). The experimental sample consisted of 80 extracted human first premolars. The sample was divided into four equal groups, and the metal brackets were bonded with different enamel pretreatments by using two adhesives: group A-10% polyacrylic acid; Fuji Ortho LC, group B-37% phosphoric acid; Fuji Ortho LC, group C-self etching primer; Transbond XT, group D-37% phosphoric acid, primer; Transbond XT. SBS of brackets was measured. After debonding of brackets, the adhesive remnant index (ARI) was evaluated. After the statistical analysis of the collected data was performed (ANOVA; Sheffe post-hoc test), the results showed that significantly lower SBS of the group B was found in relation to the groups C (p=0.031) and D (p=0.026). The results of ARI were similar in all testing groups and it was not possible to determine any statistically significant difference of the ARI (Chi- square test) between all four experimental groups. The conclusion is that the use of composite resins material with appropriate enamel pretreatment according to manufacturer's recommendation is the "gold standard" for brackets bonding for fixed orthodontic appliances.

Light Scattering based detection of food pathogens

USDA-ARS?s Scientific Manuscript database

The current methods for detecting foodborne pathogens are mostly destructive (i.e., samples need to be pretreated), and require time, personnel, and laboratories for analyses. Optical methods including light scattering based techniques have gained a lot of attention recently due to its their rapid a...

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis.

PubMed

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-05

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p=0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis

NASA Astrophysics Data System (ADS)

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-01

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4 mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p = 0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes.

Alkaline-sulfite pretreatment and use of surfactants during enzymatic hydrolysis to enhance ethanol production from sugarcane bagasse.

PubMed

Mesquita, Jéssica Faria; Ferraz, André; Aguiar, André

2016-03-01

Sugarcane bagasse is a by-product from the sugar and ethanol industry which contains approximately 70 % of its dry mass composed by polysaccharides. To convert these polysaccharides into fuel ethanol it is necessary a pretreatment step to increase the enzymatic digestibility of the recalcitrant raw material. In this work, sugarcane bagasse was pretreated by an alkaline-sulfite chemithermomechanical process for increasing its enzymatic digestibility. Na2SO3 and NaOH ratios were fixed at 2:1, and three increasing chemical loads, varying from 4 to 8 % m/m Na2SO3, were used to prepare the pretreated materials. The increase in the alkaline-sulfite load decreased the lignin content in the pretreated material up to 35.5 % at the highest chemical load. The pretreated samples presented enhanced glucose yields during enzymatic hydrolysis as a function of the pretreatment severity. The maximum glucose yield (64 %) was observed for the samples pretreated with the highest chemical load. The use of 2.5 g l(-1) Tween 20 in the hydrolysis step further increased the glucose yield to 75 %. Semi-simultaneous hydrolysis and fermentation of the pretreated materials indicated that the ethanol yield was also enhanced as a function of the pretreatment severity. The maximum ethanol yield was 56 ± 2 % for the sample pretreated with the highest chemical load. For the sample pretreated with the lowest chemical load (2 % m/m NaOH and 4 % m/m Na2SO3), adding Tween 20 during the hydrolysis process increased the ethanol yield from 25 ± 3 to 39.5 ± 1 %.

Optimization of delignification of two Pennisetum grass species by NaOH pretreatment using Taguchi and ANN statistical approach.

PubMed

Mohaptra, Sonali; Dash, Preeti Krishna; Behera, Sudhanshu Shekar; Thatoi, Hrudayanath

2016-01-01

In the bioconversion of lignocelluloses for bioethanol, pretreatment seems to be the most important step which improves the elimination of the lignin and hemicelluloses content, exposing cellulose to further hydrolysis. The present study discusses the application of dynamic statistical techniques like the Taguchi method and artificial neural network (ANN) in the optimization of pretreatment of lignocellulosic biomasses such as Hybrid Napier grass (HNG) (Pennisetum purpureum) and Denanath grass (DG) (Pennisetum pedicellatum), using alkali sodium hydroxide. This study analysed and determined a parameter combination with a low number of experiments by using the Taguchi method in which both the substrates can be efficiently pretreated. The optimized parameters obtained from the L16 orthogonal array are soaking time (18 and 26 h), temperature (60°C and 55°C), and alkali concentration (1%) for HNG and DG, respectively. High performance liquid chromatography analysis of the optimized pretreated grass varieties confirmed the presence of glucan (47.94% and 46.50%), xylan (9.35% and 7.95%), arabinan (2.15% and 2.2%), and galactan/mannan (1.44% and 1.52%) for HNG and DG, respectively. Physicochemical characterization studies of native and alkali-pretreated grasses were carried out by scanning electron microscopy and Fourier transformation Infrared spectroscopy which revealed some morphological differences between the native and optimized pretreated samples. Model validation by ANN showed a good agreement between experimental results and the predicted responses.

Optimization of enzymatic hydrolysis for ethanol production by simultaneous saccharification and fermentation of wastepaper.

PubMed

Sangkharak, Kanokphorn

2011-11-01

The present study investigated the development of high sugar production by optimization of an enzymatic hydrolysis process using both conventional and statistical methods, as well as the production of ethanol by the selected wastepaper source. Among four sources of pretreated wastepaper including office paper, newspaper, handbills and cardboard, office paper gave the highest values of cellulose (87.12%) and holocelluloses (89.07%). The effects of the amount of wastepaper, the pretreatment method and the type of enzyme on reducing sugar production from office paper were studied using conventional methods. The highest reducing sugar production (1851.28 µg L(-1); 37.03% conversion of glucose) was obtained from the optimal condition containing 40 mg of office paper, pretreated with stream explosion and hydrolysed with the combination of cellulase from Aspergillus niger and Trichoderma viride at the fixed loading rate of 20 FPU g(-1) sample. The effects of interaction of wastepaper amount and enzyme concentration as well as incubation time were studied by a statistical method using central composite design. The optimal medium composition consisted of 43.97 µg L(-1), 28.14 FPU g(-1) sample and 53.73 h of wastepaper, enzyme concentration and incubation time, respectively, and gave the highest amount of sugar production (2184.22 µg L(-1)) and percentage conversion of glucose (43.68%). The ethanol production from pretreated office paper using Saccharomyces cerevisiae in a simultaneous saccharification and fermentation process was 21.02 g L(-1) after 36 h of cultivation, corresponding to an ethanol volumetric production rate of 0.58 g ethanol L(-1) h(-1).

Microwave-Assisted Alkali Pre-Treatment, Densification and Enzymatic Saccharification of Canola Straw and Oat Hull

PubMed Central

Agu, Obiora S.; Tabil, Lope G.; Dumonceaux, Tim

2017-01-01

The effects of microwave-assisted alkali pre-treatment on pellets’ characteristics and enzymatic saccharification for bioethanol production using lignocellulosic biomass of canola straw and oat hull were investigated. The ground canola straw and oat hull were immersed in distilled water, sodium hydroxide and potassium hydroxide solutions at two concentrations (0.75% and 1.5% w/v) and exposed to microwave radiation at power level 713 W and three residence times (6, 12 and 18 min). Bulk and particle densities of ground biomass samples were determined. Alkaline-microwave pre-treated and untreated samples were subjected to single pelleting test in an Instron universal machine, pre-set to a load of 4000 N. The measured parameters, pellet density, tensile strength and dimensional stability were evaluated and the results showed that the microwave-assisted alkali pre-treated pellets had a significantly higher density and tensile strength compared to samples that were untreated or pre-treated by microwave alone. The chemical composition analysis showed that microwave-assisted alkali pre-treatment was able to disrupt and break down the lignocellulosic structure of the samples, creating an area of cellulose accessible to cellulase reactivity. The best enzymatic saccharification results gave a high glucose yield of 110.05 mg/g dry sample for canola straw ground in a 1.6 mm screen hammer mill and pre-treated with 1.5% NaOH for 18 min, and a 99.10 mg/g dry sample for oat hull ground in a 1.6 mm screen hammer mill and pre-treated with 0.75% NaOH for 18 min microwave-assisted alkali pre-treatments. The effects of pre-treatment results were supported by SEM analysis. Overall, it was found that microwave-assisted alkali pre-treatment of canola straw and oat hull at a short residence time enhanced glucose yield. PMID:28952504

Microwave-Assisted Alkali Pre-Treatment, Densification and Enzymatic Saccharification of Canola Straw and Oat Hull.

PubMed

Agu, Obiora S; Tabil, Lope G; Dumonceaux, Tim

2017-03-26

The effects of microwave-assisted alkali pre-treatment on pellets' characteristics and enzymatic saccharification for bioethanol production using lignocellulosic biomass of canola straw and oat hull were investigated. The ground canola straw and oat hull were immersed in distilled water, sodium hydroxide and potassium hydroxide solutions at two concentrations (0.75% and 1.5% w/v) and exposed to microwave radiation at power level 713 W and three residence times (6, 12 and 18 min). Bulk and particle densities of ground biomass samples were determined. Alkaline-microwave pre-treated and untreated samples were subjected to single pelleting test in an Instron universal machine, pre-set to a load of 4000 N. The measured parameters, pellet density, tensile strength and dimensional stability were evaluated and the results showed that the microwave-assisted alkali pre-treated pellets had a significantly higher density and tensile strength compared to samples that were untreated or pre-treated by microwave alone. The chemical composition analysis showed that microwave-assisted alkali pre-treatment was able to disrupt and break down the lignocellulosic structure of the samples, creating an area of cellulose accessible to cellulase reactivity. The best enzymatic saccharification results gave a high glucose yield of 110.05 mg/g dry sample for canola straw ground in a 1.6 mm screen hammer mill and pre-treated with 1.5% NaOH for 18 min, and a 99.10 mg/g dry sample for oat hull ground in a 1.6 mm screen hammer mill and pre-treated with 0.75% NaOH for 18 min microwave-assisted alkali pre-treatments. The effects of pre-treatment results were supported by SEM analysis. Overall, it was found that microwave-assisted alkali pre-treatment of canola straw and oat hull at a short residence time enhanced glucose yield.

Seasonal distribution of Legionella spp. and L. pneumophila in a river in Taiwan evaluated with culture-confirmed and direct DNA extraction methods

NASA Astrophysics Data System (ADS)

Tung, Min-Che; Chang, Tien-Yu; Hsu, Bing-Mu; Shen, Shu-Min; Huang, Jen-Te; Kao, Po-Min; Chiu, Yi-Chou; Fan, Cheng-Wei; Huang, Yu-Li

2013-07-01

In this study, we evaluated the presence and amount of Legionella in along a river in Taiwan, and the relations between seasonal distribution of Legionella spp. and geographic characteristics in the watershed were also evaluated. Water samples were pre-treated and analyzed with culture-confirmed and direct DNA extraction methods. For culture-confirmed method, water samples were cultivated through a series of selective media, and candidate colonies were confirmed by PCR. For direct DNA extraction method, direct DNA extraction was performed from pre-treated water samples. The DNA extracts were analyzed with PCR and DNA sequence analysis for species determination, quantitative PCR (qPCR) was performed to quantify Legionella concentration in the water sample. In all, 150 water samples were included in this study, with 73 (48.6%) water samples detected with Legionella spp., and 17 with L. pneumophila. Over 80% Legionella spp. detections were through direct DNA extraction method, but more than 80% L. pneumophila detections were through culture-confirmed method. While detection of Legionella spp. was done with two methods, positive results were found through only one method. Legionella spp. was detected in all seasons with detection rate ranging between 34.3-58.8% and seasonal average concentration from 1.9 × 102 to 7.1 × 103 CFU/L. Most of the L. pneumophila detections were from samples collected in fall (38.2%) and summer (6.0%), which also coincided with increased cases of Legionellosis reported through Center of Disease Control in Taiwan. The high prevalence and concentration of Legionella spp. and L. pneumophila in the surface waters should be further evaluated for potential health risks.

Quantitative Real-Time PCR Analysis of Total Propidium Monazide -Resistant Fecal Indicator Bacteria in Wastewater

EPA Science Inventory

A real-time quantitative PCR (qPCR) method and a modification of this method incorporating pretreatment of samples with propidium monoazide (PMA) were evaluated for respective analyses of total and presumptively viable Enterococcus and Bacteroidales fecal indicator bacteria. Thes...

Enhancement of high-solids enzymatic hydrolysis of corncob residues by bisulfite pretreatment for biorefinery.

PubMed

Xing, Yang; Bu, Lingxi; Zheng, Tianran; Liu, Shijie; Jiang, Jianxin

2016-12-01

Co-production of glucose, furfural and other green materials based on a lignocellulosic biorefinery is a promising way to realize the commercial application of corncob residues. An effective process was developed for glucose production using low temperature bisulfite pretreatment and high-solids enzymatic hydrolysis. Corncob residues from furfural production (FRs) were pretreated with 0.1g NaHSO 3 /g dry substrate at 100°C for 3h. Lignin was sulfonated and sulfonic groups were produced during pretreatment, which resulted in decreasing the zeta potential of the samples. Compared with raw material, bisulfite pretreatment of FRs increased the glucose yield from 18.6 to 99.45% after 72h hydrolysis at a solids loading of 12.5%. The hydrolysis residues showed a relatively high thermal stability and concentrated high derivatives. Direct pretreatment followed by enzymatic hydrolysis is an environmentally-friendly and economically-feasible method for the production of glucose and high-purity lignin, which could be further converted into high-value products. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optimization of extractants, purifying packings, and eluents for analytical extraction of organochlorine pesticides in Hydragric Acrisols.

PubMed

Zhao, Zhenhua; Xia, Liling; Wang, Fang; Jiang, Xin; Gao, Yanzheng

2012-08-01

In this study, we screened for an economic, rapid, and efficient hypotoxic pretreatment method for organochlorine pesticides in soil samples for gas chromatography (GC) analysis. The analytical extraction efficiencies of 11 different extractants, nine types of solid-phase purification (SPP) cartridge packings, and three types of eluents for 13 organochlorine pesticides (OCPs) in spiked and natural Chinese red soil (Hydragric Acrisols) were evaluated using an ultrasonic extraction and solid-phase purification method. High percent recoveries (85-106%) were obtained for the 13 organochlorine pesticides in soil when petroleum ether/acetone/water (10:5:2, v/v) was used an extractant. They were purified using celite SPP cartridge packing and eluted with 9 mL of dichloromethane/petroleum ether (1:9, v/v). The OCPs purification pretreatment of Hydragric Acrisols, using the above method, meets the GC analysis requirements. Compared with other traditional pretreatment methods for OCPs in soil samples, this method has several advantages, such as a short extraction time, reducing the amount of solvent, having no emulsion phenomenon, and hypotoxicity to the laboratory technicians. The concentrations of 1,1,1,-trichloro-2(p-chlorophenyl)-2-(o-chlorophenyl) ethane (DDTs; 3.42-8.08 ng g(-1)) in field soils were higher than the hexachlorocyclohexane concentration (2.94-6.12 ng g(-1)). The 1,1-dichloro-2,2-bis(p-chlorophenyl) ethylene (p,p'-DDE) + 1,1-dichloro-2,2-bis(p-chlorophenyl)-ethane (p,p'-DDD)/p,p'-DDT ratio in this field soil was approximately 2.7, suggesting that no new DDT pollution source was introduced into the sampling site.

Effect of iron salt type and dosing mode on Fenton-based pretreatment of rice straw for enzymatic hydrolysis.

PubMed

Gan, Yu-Yan; Zhou, Si-Li; Dai, Xiao; Wu, Han; Xiong, Zi-Yao; Qin, Yuan-Hang; Ma, Jiayu; Yang, Li; Wu, Zai-Kun; Wang, Tie-Lin; Wang, Wei-Guo; Wang, Cun-Wen

2018-06-15

Fenton-based processes with four different iron salts in two different dosing modes were used to pretreat rice straw (RS) samples to increase their enzymatic digestibility. The composition analysis shows that the RS sample pretreated by the dosing mode of iron salt adding into H 2 O 2 has a much lower hemicellulose content than that pretreated by the dosing mode of H 2 O 2 adding into iron salt, and the RS sample pretreated by the chloride salt-based Fenton process has a much lower lignin content and a slightly lower hemicellulose content than that pretreated by the sulphate salt-based Fenton process. The higher concentration of reducing sugar observed on the RS sample with lower lignin and hemicellulose contents justifies that the Fenton-based process could enhance the enzymic hydrolysis of RS by removing hemicellulose and lignin and increasing its accessibility to cellulase. FeCl 3 ·6H 2 O adding into H 2 O 2 is the most efficient Fenton-based process for RS pretreatment. Copyright © 2018 Elsevier Ltd. All rights reserved.

Direct determination and speciation of mercury compounds in environmental and biological samples by carbon bed atomic absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skelly, E.M.

A method was developed for the direct determination of mercury in water and biological samples using a unique carbon bed atomizer for atomic absorption spectroscopy. The method avoided sources of error such as loss of volatile mercury during sample digestion and contamination of samples through added reagents by eliminating sample pretreatment steps. The design of the atomizer allowed use of the 184.9 nm mercury resonance line in the vacuum ultraviolet region, which increased sensitivity over the commonly used spin-forbidden 253.7 nm line. The carbon bed atomizer method was applied to a study of mercury concentrations in water, hair, sweat, urine,more » blood, breath and saliva samples from a non-occupationally exposed population. Data were collected on the average concentration, the range and distribution of mercury in the samples. Data were also collected illustrating individual variations in mercury concentrations with time. Concentrations of mercury found were significantly higher than values reported in the literature for a ''normal'' population. This is attributed to the increased accuracy gained by eliminating pretreatment steps and increasing atomization efficiency. Absorption traces were obtained for various solutions of pure and complexed mercury compounds. Absorption traces of biological fluids were also obtained. Differences were observed in the absorption-temperatures traces of various compounds. The utility of this technique for studying complexation was demonstrated.« less

Evaluation of electricity generation from ultrasonic and heat/alkaline pretreatment of different sludge types using microbial fuel cells.

PubMed

Oh, Sang-Eun; Yoon, Joung Yee; Gurung, Anup; Kim, Dong-Jin

2014-08-01

This study investigated the effects of different sludge pretreatment methods (ultrasonic vs. combined heat/alkali) with varied sources of municipal sewage sludge (primary sludge (PS), secondary excess sludge (ES), anaerobic digestion sludge (ADS)) on electricity generation in microbial fuel cells (MFCs). Introduction of ultrasonically pretreated sludge (PS, ES, ADS) to MFCs generated maximum power densities of 13.59, 9.78 and 12.67mW/m(2) and soluble COD (SCOD) removal efficiencies of 87%, 90% and 57%, respectively. The sludge pretreated by combined heat/alkali (0.04N NaOH at 120°C for 1h) produced maximum power densities of 10.03, 5.21 and 12.53mW/m(2) and SCOD removal efficiencies of 83%, 75% and 74% with PS, ES and ADS samples, respectively. Higher SCOD by sludge pretreatment enhanced performance of the MFCs and the electricity generation was linearly proportional to the SCOD removal, especially for ES. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biological abatement of cellulase inhibitors.

PubMed

Cao, Guangli; Ximenes, Eduardo; Nichols, Nancy N; Zhang, Leyu; Ladisch, Michael

2013-10-01

Removal of enzyme inhibitors released during lignocellulose pretreatment is essential for economically feasible biofuel production. We tested bio-abatement to mitigate enzyme inhibitor effects observed in corn stover liquors after pretreatment with either dilute acid or liquid hot water at 10% (w/v) solids. Bio-abatement of liquors was followed by enzymatic hydrolysis of cellulose. To distinguish between inhibitor effects on enzymes and recalcitrance of the substrate, pretreated corn stover solids were removed and replaced with 1% (w/v) Solka Floc. Cellulose conversion in the presence of bio-abated liquors from dilute acid pretreatment was 8.6% (0.1x enzyme) and 16% (1x enzyme) higher than control (non-abated) samples. In the presence of bio-abated liquor from liquid hot water pretreated corn stover, 10% (0.1x enzyme) and 13% (1x enzyme) higher cellulose conversion was obtained compared to control. Bio-abatement yielded improved enzyme hydrolysis in the same range as that obtained using a chemical (overliming) method for mitigating inhibitors. Copyright © 2013 Elsevier Ltd. All rights reserved.

Development of andrographolide molecularly imprinted polymer for solid-phase extraction

NASA Astrophysics Data System (ADS)

Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

2011-06-01

A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions.

PubMed

Satínský, Dalibor; Havlíková, Lucie; Solich, Petr

2013-08-01

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min(-1) and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5% triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min(-1) and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL(-1).

Effect of pretreatment on rehydration, colour and nanoindentation properties of potato cylinders dried using a mixed-mode solar dryer.

PubMed

Dhalsamant, Kshanaprava; Tripathy, Punyadarshini P; Shrivastava, Shanker L

2017-08-01

Desirable quality estimation is an important consumer driver for wider acceptability of mixed-mode solar drying of potatoes in food industries. The aim of this study is to characterise rehydration, colour, texture, nanoindentaion and microstructure of dried potato samples and to establish the influence of pre-drying treatment on the above qualities. The water absorption capacity and rehydration ability of solar dried potato were significantly influenced by pretreatment followed by rehydration temperature and sample diameter. The redness index (a*) of pretreated dried samples was lower with simultaneous higher value of yellowness index (b*), chroma (C*) and hue angle (h*). Also, the average nanohardness (H) of pretreated samples increased significantly by 22.64% compared to that of untreated samples. The average reduced modulus (E r ) and Young's modulus (E s ) of dried potato samples were 1.865 GPa and 1.403 GPa, respectively. Moreover, creep displacement of 43.27 nm was traced in the untreated potato samples during a 20 s dwell time under a constant load of 200 µN in the nanoindentation test. Micrographs revealed more uniform pore spaces in pretreated samples. Pretreated, thinner potato samples achieved better quality dried products in terms of rehydration, colour, texture and nanohardness indices with significantly improved microstructure and creep resistance properties. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

[Simultaneous determination of 22 typical pharmaceuticals and personal care products in environmental water using ultra performance liquid chromatography- triple quadrupole mass spectrometry].

PubMed

Wu, Chunying; Gu, Feng; Bai, Lu; Lu, Wenlong

2015-08-01

An analytical method for simultaneous determination of 22 typical pharmaceuticals and personal care products (PPCPs) in environmental water samples was developed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). An Oasis HLB solid phase extraction cartridge, methanol as washing solution, water containing 0. 1% formic acid-methanol (7:3, v/v) as the mobile phases were selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 73% to 125% in water with the relative standard deviations ( RSDs) from 8.8% to 17.5%, and the linear ranges were from 2 to 2 000 µg/L with correlation coefficients (R2) not less than 0.997. The method can be applied to simultaneous determination of the 22 typical PPCPs in environmental water samples because of its low detection limits and high recoveries. It can provide support and help for the related research on water environmental risk assessment and control of the micro-organic pollutants.

Quantitative (13)C MultiCP solid-state NMR as a tool for evaluation of cellulose crystallinity index measured directly inside sugarcane biomass.

PubMed

Bernardinelli, Oigres Daniel; Lima, Marisa Aparecida; Rezende, Camila Alves; Polikarpov, Igor; deAzevedo, Eduardo Ribeiro

2015-01-01

The crystallinity index (CI) is often associated with changes in cellulose structure after biological and physicochemical pretreatments. While some results obtained with lignocellulosic biomass demonstrate a progressive increase in the CI as a function of pretreatments, it is also shown that the CI can significantly vary depending on the choice of the measurement method. Besides, the influence of the CI on the recalcitrance of biomass has been controversial for a long time, but the most recent results tend to point out that the efficiency of pretreatments in reducing the recalcitrance is not clearly correlated with the decrease of the CI. Much of this controversy is somewhat associated with the inability to distinguish between the CI of the cellulose inside the biomass and the CI of the full biomass, which contains other amorphous components such as lignin and hemicellulose. Cross polarization by multiple contact periods (Multi-CP) method was used to obtain quantitative (13)C solid-state nuclear magnetic resonance (ssNMR) spectra of sugarcane bagasse biomass submitted to two-step pretreatments and/or enzymatic hydrolysis. By comparing the dipolar filtered Multi-CP (13)C NMR spectra of untreated bagasse samples with those of samples submitted to acid pretreatment, we show that a 1% H2SO4-assisted pretreatment was very effective in removing practically all the hemicellulose signals. This led us to propose a spectral editing procedure based on the subtraction of MultiCP spectra of acid-treated biomass from that of the extracted lignin, to obtain a virtually pure cellulose spectrum. Based on this idea, we were able to evaluate the CI of the native cellulose inside the sugarcane bagasse biomass. The results show the validity of the proposed method as a tool for evaluating the variations in the CI of the cellulose inside biomasses of similar kinds. Despite a clear increase in the CI of biomass as measured by X-ray diffraction, no significant variations were observed in the CI of the cellulose inside the biomass after a particular 1% H2SO4/0.25-4% NaOH chemical-assisted pretreatments. The CI of cellulose inside the biomass solid fraction that remained after the enzymatic hydrolysis was also evaluated. The results show a slight increase in crystallinity.

Multi-pesticides residue analysis of grains using modified magnetic nanoparticle adsorbent for facile and efficient cleanup.

PubMed

Liu, Zhenzhen; Qi, Peipei; Wang, Xiangyun; Wang, Zhiwei; Xu, Xiahong; Chen, Wenxue; Wu, Liyu; Zhang, Hu; Wang, Qiang; Wang, Xinquan

2017-09-01

A facile, rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis of grains. Magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane (Fe 3 O 4 -PSA) and commercial C18 were selected as the cleanup adsorbents to remove the target interferences of the matrix, such as fatty acids and non-polar compounds. Rice was used as the representative grain sample for method optimization. The amount of Fe 3 O 4 -PSA and C18 were systematically investigated for selecting the suitable purification conditions, and the simultaneous determination of 50 pesticides and 8 related metabolites in rice was established by liquid chromatography-tandem mass spectrometry. Under the optimal conditions, the method validation was performed including linearity, sensitivity, matrix effect, recovery and precision, which all satisfy the requirement for pesticides residue analysis. Compared to the conventional QuEChERS method with non-magnetic material as cleanup adsorbent, the present method can save 30% of the pretreatment time, giving the high throughput analysis possible. Copyright © 2017 Elsevier Ltd. All rights reserved.

A study on characteristic of different sample pretreatment methods to evaluate the entrapment efficiency of liposomes.

PubMed

Ran, Congcong; Chen, Dan; Xu, Meng; Du, Chaohui; Li, Qinglian; Jiang, Ye

2016-08-15

To examine how methods affect the evaluation of entrapment efficiency (EE) of liposomes, four different sample pretreatment methods were adopted in the experiment. The four sample pretreatment methods were size-exclusion chromatography (SEC), solid-phase extraction (SPE), centrifugation ultrafiltration (CF-UF) and hollow fiber centrifugal ultrafiltration (HF-CF-UF). Amphotericin B (AmB), which could self-associate to form aggregates in water is adopted as the model drugs in this paper. In the present work, it was found that the characterization results of four methods were quite different. The EE of liposome by SEC was about 93%, only 5-13% using C18 or HLB columns, and approximately 100% by CF-UF. The EE of HF-CF-UF reached up to nearly 99.0%. Further, this paper revealed the reasons making the difference of EE among four methods. Conventional SEC may distort the authentic of EE of liposomes with mainly employing some small liposomes or excessive water as eluent. For SPE, cholesterol on liposome surface could interact with the stationary phase making it hard to elute with water, and increase the risk of liposome leakage. While for CF-UF, concentration polarization was a main limitation hindering unentrapped drug to pass through membrane, making unentrapped drug undetectable in liposome. HF-CF-UF could truly reflect EE of liposomes with the concentration of unentrapped AmB lower than 25.0μg/mL. However, when the concentration was higher than 25.0μg/mL, AmB aggregates could be entrapped by hollow fiber. From the above analysis, this paper came to the conclusion that each method had its own feature in characterization. This study provided a reasonable guideline for choosing methods to character the EE of liposome. Copyright © 2016 Elsevier B.V. All rights reserved.

Interface actions between TiO2 and porous diatomite on the structure and photocatalytic activity of TiO2-diatomite

NASA Astrophysics Data System (ADS)

Xia, Yue; Li, Fangfei; Jiang, Yinshan; Xia, Maosheng; Xue, Bing; Li, Yanjuan

2014-06-01

TiO2-diatomite photocatalysts were prepared by sol-gel process with various pre-modified diatomite. In order to obtain diatomite with different surface characteristics, two modification approaches including calcination and phosphoric acid treatment on the micro-structure of diatomite are introduced. The photocatalysts were characterized by XRD, XPS, nitrogen adsorption-desorption isotherms and micromorphology analysis. The results indicate that, compared with pure TiO2, the anatase-to-rutile phase transition temperature of TiO2 loaded on diatomite carrier is significantly increased to nearly 900 °C, depending on the different pretreatment method of diatomite. The photocatalytic activities of different samples were evaluated by their degradation rate of methyl orange (MO) dye under UV and visible-light irradiation. The samples prepared by phosphoric acid pretreatment method exhibit the highest photocatalytic activity. After 90 min of UV irradiation, about 90% of MO is decomposed by the best effective photocatalyst. And after 8 h visible-light irradiation, nearly 60% of MO is decomposed by the same sample. Further mechanism investigation reveals that the H3PO4 pretreatment process can obviously change the surface features of diatomite carrier, cause the formation of Si-O-Ti bond, increase the binding strength between TiO2 and diatomite, restrain crystal growth of loaded TiO2, and thus form thermal-stable mesoporous structure at the granular spaces. It helps to build micro-, meso- and macro-porous hierarchical porous structure in TiO2-diatomite, and improves the charge and mass transfer efficiency during catalyzing process, resulting in the significantly increased photocatalytic activity of TiO2-diatomite pretreated by phosphoric acid.

Chemical and morphological characterization of sugarcane bagasse submitted to a delignification process for enhanced enzymatic digestibility

PubMed Central

2011-01-01

Background In recent years, biorefining of lignocellulosic biomass to produce multi-products such as ethanol and other biomaterials has become a dynamic research area. Pretreatment technologies that fractionate sugarcane bagasse are essential for the successful use of this feedstock in ethanol production. In this paper, we investigate modifications in the morphology and chemical composition of sugarcane bagasse submitted to a two-step treatment, using diluted acid followed by a delignification process with increasing sodium hydroxide concentrations. Detailed chemical and morphological characterization of the samples after each pretreatment condition, studied by high performance liquid chromatography, solid-state nuclear magnetic resonance, diffuse reflectance Fourier transformed infrared spectroscopy and scanning electron microscopy, is reported, together with sample crystallinity and enzymatic digestibility. Results Chemical composition analysis performed on samples obtained after different pretreatment conditions showed that up to 96% and 85% of hemicellulose and lignin fractions, respectively, were removed by this two-step method when sodium hydroxide concentrations of 1% (m/v) or higher were used. The efficient lignin removal resulted in an enhanced hydrolysis yield reaching values around 100%. Considering the cellulose loss due to the pretreatment (maximum of 30%, depending on the process), the total cellulose conversion increases significantly from 22.0% (value for the untreated bagasse) to 72.4%. The delignification process, with consequent increase in the cellulose to lignin ratio, is also clearly observed by nuclear magnetic resonance and diffuse reflectance Fourier transformed infrared spectroscopy experiments. We also demonstrated that the morphological changes contributing to this remarkable improvement occur as a consequence of lignin removal from the sample. Bagasse unstructuring is favored by the loss of cohesion between neighboring cell walls, as well as by changes in the inner cell wall structure, such as damaging, hole formation and loss of mechanical resistance, facilitating liquid and enzyme access to crystalline cellulose. Conclusions The results presented herewith show the efficiency of the proposed method for improving the enzymatic digestibility of sugarcane bagasse and provide understanding of the pretreatment action mechanism. Combining the different techniques applied in this work warranted thorough information about the undergoing morphological and chemical changes and was an efficient approach to understand the morphological effects resulting from sample delignification and its influence on the enhanced hydrolysis results. PMID:22122978

Enhancement of drying and rehydration characteristics of okra by ultrasound pre-treatment application

NASA Astrophysics Data System (ADS)

Tüfekçi, Senem; Özkal, Sami Gökhan

2017-07-01

Effect of ultrasound application prior to hot air drying on drying and rehydration kinetics, rehydration ratio and microstructure of okra slices were investigated. For this purpose, the selected parameters are ultrasound pre-treatment time (10, 20 and 30 min), ultrasound amplitude (55 and 100%) and the temperature of drying air (60 and 70 °C). 5 mm thick cylindrical shaped okra slices were used in the experiments. The samples were immersed in water and ultrasonic pre-treatments were done in water with ultrasonic probe connected to an ultrasonic generator with 20 kHz frequency. Pre-treated samples were dried in a tray drier with a 0.3 m/s air velocity. Ultrasound pre-treatment affected the drying rate of the okra slices significantly. Drying time of okra slices was decreased by the application of ultrasound pre-treatment. Modified Page model found to be the most suitable model for describing the drying characteristics of okra slices. Improvements in rehydration properties of the dried samples were observed due to the ultrasound pre-treatment. The influence of the ultrasound pre-treatment on microstructure was clearly observed through scanning electron microscopy images of the dried samples. As the amplitude of ultrasound increased the changes in structure of the okra tissue increased.

[Comparative study on five pretreatment methods for ICP-OES determination of mineral elements in Rosa rugosa].

PubMed

Zhao, Ning; Yang, Bin; Duan, Yu-Cen; Lei, Ran

2011-08-01

Abstract Five different pretreatment methods, including dry ashing and microwave digestion with four acid systems (HNO3 + H2O2, HNO3 + H2O2 + HF, HNO3 + HClO4 and HNO3 + HClO4 + HF), were employed for digestion of the samples of Rosa rugosa. Nine major and trace elements were determined using ICP-OES method. The addition standard recovery rates indicate that, with the system of HNO3 + HClO4, better results can be obtained for most of the determined elements. With this method, except for Fe, the recovery rates are in the range of 95.4%-104.6%. For Fe, higher recovery rate (99%) was obtained with HNO3 + H2O2 + HF system.

Pretreatment to avoid positive RT-PCR results with inactivated viruses.

PubMed

Nuanualsuwan, Suphachai; Cliver, Dean O

2002-07-01

Enteric viruses that are important causes of human disease must often be detected by reverse transcription-polymerase chain reaction (RT-PCR), a method that commonly yields positive results with samples that contain only inactivated virus. This study was intended to develop a pretreatment for samples, so that inactivated viruses would not be detected by the RT-PCR procedure. Model viruses were human hepatitis A virus, vaccine poliovirus 1 and feline calicivirus as a surrogate for the Norwalk-like viruses. Each virus was inactivated (from an initial titer of approximately 10(3) PFU/ml) by ultraviolet light, hypochlorite or heating at 72 degrees C. Inactivated viruses, that were treated with proteinase K and ribonuclease for 30 min at 37 degrees C before RT-PCR, gave a negative result, which is to say that no amplicon was detected after the reaction was completed. This antecedent to the RT-PCR method may be applicable to other types of viruses, to viruses inactivated in other ways and to other molecular methods of virus detection.

Identifying moderators of the adherence-outcome relation in cognitive therapy for depression.

PubMed

Sasso, Katherine E; Strunk, Daniel R; Braun, Justin D; DeRubeis, Robert J; Brotman, Melissa A

2015-10-01

Little is known about the influence of patients' pretreatment characteristics on the adherence-outcome relation in cognitive therapy (CT) for depression. In a sample of 57 depressed adults participating in CT, the authors examined interactions between pretreatment patient characteristics and therapist adherence in predicting session-to-session symptom change. Using items from the Collaborative Study Psychotherapy Rating Scale, the authors assessed 3 facets of therapist adherence: cognitive methods, negotiating/structuring, and behavioral methods/homework. Two graduate students rated Sessions 1-4 for adherence. Symptoms were assessed prior to each session with the Beck Depression Inventory-II. Moderators were assessed as part of patients' intake evaluations. After correcting for multiple comparisons, patient gender remained a significant moderator of the relationship between cognitive methods and next-session symptom change; cognitive methods more strongly predicted greater symptom improvement for women as compared to men. Pretreatment anxiety and number of prior depressive episodes were significant moderators of the relationship between behavioral methods/homework and next-session symptom change, with greater behavioral methods/homework predicting symptom improvement more strongly among patients high in pretreatment anxiety and among patients with relatively few prior depressive episodes. This is the first study to provide evidence of how therapist adherence is differentially related to outcome among depressed patients with different characteristics. If replicated, these findings may inform clinical decisions regarding the use of specific facets of adherence in CT for depression with specific patients. (c) 2015 APA, all rights reserved).

Pretreatment of paper tube residuals for improved biogas production.

PubMed

Teghammar, Anna; Yngvesson, Johan; Lundin, Magnus; Taherzadeh, Mohammad J; Horváth, Ilona Sárvári

2010-02-01

Paper tube residuals, which are lignocellulosic wastes, have been studied as substrate for biogas (methane) production. Steam explosion and nonexplosive hydrothermal pretreatment, in combination with sodium hydroxide and/or hydrogen peroxide, have been used to improve the biogas production. The treatment conditions of temperature, time and addition of NaOH and H(2)O(2) were statistically evaluated for methane production. Explosive pretreatment was more successful than the nonexplosive method, and gave the best results at 220 degrees C, 10 min, with addition of both 2% NaOH and 2% H(2)O(2). Digestion of the pretreated materials at these conditions yielded 493 N ml/g VS methane which was 107% more than the untreated materials. In addition, the initial digestion rate was improved by 132% compared to the untreated samples. The addition of NaOH was, besides the explosion effect, the most important factor to improve the biogas production.

Effect of different pretreatments on dried chilli (Capsicum annum L.) quality

NASA Astrophysics Data System (ADS)

Anoraga, S. B.; Sabarisman, I.; Ainuri, M.

2018-03-01

Chilli (Capsicum annum L.) has significant price fluctuation. When the chilli price is declined, it causes food waste from unsold chilli. Therefore, drying chilli is a solution for this condition. Futhermore, it can be processed for various product like chilli powder, chilli sauce, etc. The aim of this study was to investigate the effect of different pretreatments on dried chilli quality. Chilli was blenched with hot water and steam before drying. The purpose of this pretreatments is to inactivate enzyme that prevents color and vitamin C losses. The quality parameters were moisture content, colour, vitamin C content, and capsaicin. Changes were observed by gravimetri method for moisture content, chromameter in L* a * b * colour model, and iodine titration for vitamin C. After drying for 20 hours at 60°C, chilli with steam blanching pretreatment dried rapidly than other samples. Unpretreated chilli had higher vitamin C content and better color than blanched chilli.

Determination of novel brominated flame retardants and polybrominated diphenyl ethers in serum using gas chromatography-mass spectrometry with two simplified sample preparation procedures.

PubMed

Gao, Le; Li, Jian; Wu, Yandan; Yu, Miaohao; Chen, Tian; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei

2016-11-01

Two simple and efficient pretreatment procedures have been developed for the simultaneous extraction and cleanup of six novel brominated flame retardants (NBFRs) and eight common polybrominated diphenyl ethers (PBDEs) in human serum. The first sample pretreatment procedure was a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach. An acetone/hexane mixture was employed to isolate the lipid and analytes from the serum with a combination of MgSO 4 and NaCl, followed by a dispersive solid-phase extraction (d-SPE) step using C18 particles as a sorbent. The second sample pretreatment procedure was based on solid-phase extraction. The sample extraction and cleanup were conducted directly on an Oasis HLB SPE column using 5 % aqueous isopropanol, concentrated sulfuric acid, and 10 % aqueous methanol, followed by elution with dichloromethane. The NBFRs and PBDEs were then detected using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI MS). The methods were assessed for repeatability, accuracy, selectivity, limits of detection (LODs), and linearity. The results of spike recovery experiments in fetal bovine serum showed that average recoveries ranged from 77.9 % to 128.8 % with relative standard deviations (RSDs) from 0.73 % to 12.37 % for most of the analytes. The LODs for the analytes in fetal bovine serum ranged from 0.3 to 50.8 pg/mL except for decabromodiphenyl ethane. The proposed method was successfully applied to the determination of the 14 brominated flame retardants in human serum. The two pretreatment procedures described here are simple, accurate, and precise, and are suitable for the routine analysis of human serum. Graphical Abstract Workflow of a QuEChERS-based approach (top) and an SPE-based approach (bottom) for the detection of PBDEs and NBFRs in serum.

Effect of laser and air abrasion pretreatment on the microleakage of a fissure sealant applied with conventional and self etch adhesives.

PubMed

Tirali, R E; Celik, C; Arhun, N; Berk, G; Cehreli, S B

2013-01-01

The purpose of this study was to investigate the effects of different pretreatment protocols along with different bonding agents on the microleakage of a fissure sealant material. A total of 144 freshly extracted noncarious human third molars were used The teeth were randomly assigned into three groups with respect to the pretreatment protocol employed: A. Air Abrasion B. Er,Cr:YSGG laser C. No pretreatment (Control). In each group specimens were further subjected to one of the following procedures before application of the sealant: 1. %36 Phosphoric acid-etch (AE) (DeTrey Conditioner 36/Denstply, UK) 2.AE+Prime&Bond NT (Dentsply, UK) 3. Clearfil S3 Bond (Kuraray, Japan) 4. Clearfil SE Bond (Kuraray, Japan). All teeth were sealed with the same fissure sealant material (Conseal F/SDI, Australia). Sealed teeth were further subjected to thermocycling, dye penetration test, sectioning and quantitative image analysis. Statistical evaluation of the microleakage data was performed with two way independent ANOVA and multiple comparisons test at p = 0.05. For qualitative evaluation 2 samples from each group were examined under Scanning Electron Microscopy. Microleakage was affected by both the type of pretreatment and the subsequent bonding protocols employed (p < 0.05). Overall, the highest (Mean = 0.36 mm) and lowest (Mean = 0.06 mm) microleakage values were observed in samples with unpretreated enamel sealed by S3+Conseal F and samples with laser pretreated enamel sealed by Acid Etch+Prime&-Bond+Conseal F protocols, respectively (p < 0.05). In the acid-etch group samples pretreated with laser yielded in slightly lower microleakage scores when compared with unpretreated samples and samples pretreated with air abrasion but the statistical significance was not important (p = 0,179). Similarly, when bonding agent is applied following acid-etching procedure, microleakage scores were not affected from pretreatment protocol (p = 0,615) (intact enamel/laser or air-abrasion). For both all-in one and two step self etch adhesive systems, unpretreated samples demonstrated the highest microleakage scores. For the groups in which bonding agent was utilized, pretreatments did not effected microleakage. Both the tested pretreatment protocols and adhesive procedures had different effects on the sealing properties of Conseal F in permanent tooth enamel.

Extraction of valuable compounds from mangosteen pericarps by hydrothermal assisted sonication

NASA Astrophysics Data System (ADS)

Machmudah, Siti; Lestari, Sarah Duta; Shiddiqi, Qifni Yasa'Ash; Widiyastuti, Winardi, Sugeng; Wahyudiono, Kanda, Hideki; Goto, Motonobu

2015-12-01

Valuable compounds, such as xanthone and phenolic compounds, from mangosteen pericarps was extracted by hydrothermal treatment at temperatures of 120-160 °C and pressures of 5 MPa using batch and semi-batch extractor. This method is a simple and environmentally friendly extraction method requiring no chemicals other than water. Under these conditions, there is possibility for the formation of phenolic compounds from mangosteen pericarps from decomposition of bounds between lignin, cellulose, and hemicellulose via autohydrolysis. In order to increase the amount of extracted valuable compounds, sonication pre-treament was performed prior to the hydrothermal extraction process. 30 min of sonication pre-treatment could increase significantly the amount of xanthone and phenolic compounds mangosteen pericarps extraction. In batch-system, the xanthone recovery approach to 100 % at 160 °C with 30 min sonication pre-treatment for 150 min extraction time. Under semi-batch process, the total phenolic compounds in the extract was 217 mg/g sample at 160 °C with 30 min sonication pre-treatment for 150 min total extraction time. The results revealed that hydrothermal extraction assisted sonication pre-treatment is applicable method for the isolation of polyphenolic compounds from other types of biomass and may lead to an advanced plant biomass components extraction technology.

A comparative study of ultrasonication, Fenton's oxidation and ferro-sonication treatment for degradation of carbamazepine from wastewater and toxicity test by Yeast Estrogen Screen (YES) assay.

PubMed

Mohapatra, D P; Brar, S K; Tyagi, R D; Picard, P; Surampalli, R Y

2013-03-01

A comparative study of ultrasonication (US), Fenton's oxidation (FO) and ferro-sonication (FS) (combination of ultrasonication and Fenton's oxidation) advanced oxidation processes (AOPs) for degradation of carbamazepine (CBZ) from wastewater (WW) is reported for the first time. CBZ is a worldwide used antiepileptic drug, found as a persistent emerging contaminant in many wastewater treatment plants (WWTPs) effluents and other aquatic environments. The oxidation treatments of WW caused an effective removal of the drug. Among the various US, FO and FS pre-treatments carried out, higher soluble chemical oxygen demand (SCOD) and soluble organic carbon (SOC) increment (63 to 86% and 21 to 34%, respectively) was observed during FO pre-treatment process, resulting in higher removal of CBZ (84 to 100%) from WW. Furthermore, analysis of by-products formed during US, FO and FS pre-treatment in WW was carried out by using laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). LDTD-APCI-MS/MS analysis indicated formation of two by-products, such as epoxycarbamazepine and hydroxycarbamazepine due to the reaction of hydroxyl radicals (OH) with CBZ during the three types of pre-treatment processes. In addition, the estrogenic activity of US, FO and FS pre-treated sample with CBZ and its by-products was carried out by Yeast Estrogen Screen (YES) assay method. Based upon the YES test results, none of the pre-treated samples showed estrogenic activity. Copyright © 2012 Elsevier B.V. All rights reserved.

Microbiological test results using three urine pretreatment regimes with 316L stainless steel

NASA Technical Reports Server (NTRS)

Huff, Timothy L.

1993-01-01

Three urine pretreatments, (1) Oxone (Dupont) and sulfuric acid, (2) sodium hypochlorite and sulfuric acid, (3) and ozone, were studied for their ability to reduce microbial levels in urine and minimize surface attachment to 316L stainless steel coupons. Urine samples inoculated with Bacillus insolitus and a filamentous mold, organisms previously recovered from the vapor compression distillation subsystem of NASA Space Station Freedom water recovery test were tested in glass corrosion cells containing base or weld metal coupons. Microbial levels, changes in pH, color, turbidity, and odor of the fluid were monitored over the course of the 21-day test. Specimen surfaces were examined by scanning electron microscopy at completion of the test for microbial attachment. Ozonated urine samples were less turbid and had lower microbial levels than controls or samples receiving other pretreatments. Base metal coupons receiving pretreatment were relatively free of attached bacteria. However, well-developed biofilms were found in the heat-affected regions of welded coupons receiving Oxone and hypochlorite pretreatments. Few bacteria were observed in the same regions of the ozone pretreatment sample.

Controllable synthesis of (NH4)Fe2(PO4)2(OH)·2H2O using two-step route: Ultrasonic-intensified impinging stream pre-treatment followed by hydrothermal treatment.

PubMed

Dong, Bin; Li, Guang; Yang, Xiaogang; Chen, Luming; Chen, George Z

2018-04-01

(NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O samples with different morphology are successfully synthesized via two-step synthesis route - ultrasonic-intensified impinging stream pre-treatment followed by hydrothermal treatment (UIHT) method. The effects of the adoption of ultrasonic-intensified impinging stream pre-treatment, reagent concentration (C), pH value of solution and hydrothermal reaction time (T) on the physical and chemical properties of the synthesised (NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O composites and FePO 4 particles were systematically investigated. Nano-seeds were firstly synthesized using the ultrasonic-intensified T-mixer and these nano-seeds were then transferred into a hydrothermal reactor, heated at 170 °C for 4 h. The obtained samples were characterized by utilising XRD, BET, TG-DTA, SEM, TEM, Mastersizer 3000 and FTIR, respectively. The experimental results have indicated that the particle size and morphology of the obtained samples are remarkably affected by the use of ultrasonic-intensified impinging stream pre-treatment, hydrothermal reaction time, reagent concentration, and pH value of solution. When such (NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O precursor samples were transformed to FePO 4 products after sintering at 650 °C for 10 h, the SEM images have clearly shown that both the precursor and the final product still retain their monodispersed spherical microstructures with similar particle size of about 3 μm when the samples are synthesised at the optimised condition. Copyright © 2017 Elsevier B.V. All rights reserved.

Influence of twin-screw extrusion on soluble arabinoxylans and corn fiber gum from corn fiber.

PubMed

Singkhornart, Sasathorn; Lee, Seul Gi; Ryu, Gi Hyung

2013-09-01

The effect of feed moisture content and screw speed in the extrusion process with and without chemical pretreatment of corn fiber was investigated. Different chemical pretreatment methods (NaOH and H2 SO4 solution) were compared. The improvement of reducing sugar, soluble arabinoxylans (SAX) content and the yield of corn fiber gum was measured. A high reducing sugar content was obtained in the filtrate fraction from the extruded destarched corn fiber (EDCF) with H₂SO₄ pretreatment. Feed moisture content most effectively improved both reducing sugar and SAX content of filtrate. Increasing feed moisture content and screw speed resulted in a higher SAX content in the filtrate of the EDCF with NaOH pretreatment. The SAX content of the residual solid from the EDCF with NaOH pretreatment was higher compared to H₂SO₄ pretreated and unpretreated samples and significantly increased with decreasing feed moisture content. The screw speed did not have a major impact after enzyme hydrolysis. The yield of corn fiber gum was increased by 12% using NaOH pretreatment combined with extrusion process as compared to the destarched corn fiber. The results show the great potential of the extrusion process as an effective pretreatment for disruption the lignocelluloses of corn fiber, leading to conversion of cellulose to glucose and hemicelluloses to SAX and isolation of corn fiber gum. © 2013 Society of Chemical Industry.

[Detection of Hawthorn Fruit Defects Using Hyperspectral Imaging].

PubMed

Liu, De-hua; Zhang, Shu-juan; Wang, Bin; Yu, Ke-qiang; Zhao, Yan-ru; He, Yong

2015-11-01

Hyperspectral imaging technology covered the range of 380-1000 nm was employed to detect defects (bruise and insect damage) of hawthorn fruit. A total of 134 samples were collected, which included damage fruit of 46, pest fruit of 30, injure and pest fruit of 10 and intact fruit of 48. Because calyx · s⁻¹ tem-end and bruise/insect damage regions offered a similar appearance characteristic in RGB images, which could produce easily confusion between them. Hence, five types of defects including bruise, insect damage, sound, calyx, and stem-end were collected from 230 hawthorn fruits. After acquiring hyperspectral images of hawthorn fruits, the spectral data were extracted from region of interest (ROI). Then, several pretreatment methods of standard normalized variate (SNV), savitzky golay (SG), median filter (MF) and multiplicative scatter correction (MSC) were used and partial least squares method(PLS) model was carried out to obtain the better performance. Accordingly to their results, SNV pretreatment methods assessed by PLS was viewed as best pretreatment method. Lastly, SNV was chosen as the pretreatment method. Spectral features of five different regions were combined with Regression coefficients(RCs) of partial least squares-discriminant analysis (PLS-DA) model was used to identify the important wavelengths and ten wavebands at 483, 563, 645, 671, 686, 722, 777, 819, 837 and 942 nm were selected from all of the wavebands. Using Kennard-Stone algorithm, all kinds of samples were randomly divided into training set (173) and test set (57) according to the proportion of 3:1. And then, least squares-support vector machine (LS-SVM) discriminate model was established by using the selected wavebands. The results showed that the discriminate accuracy of the method was 91.23%. In the other hand, images at ten important wavebands were executed to Principal component analysis (PCA). Using "Sobel" operator and region growing algrorithm "Regiongrow", the edge and defect feature of 86 Hawthorn could be recognized. Lastly, the detect precision of bruised, insect damage and two-defect samples is 95.65%, 86.67% and 100%, respectively. This investigation demonstrated that hyperspectral imaging technology could detect the defects of bruise, insect damage, calyx, and stem-end in hawthorn fruit in qualitative analysis and feature detection which provided a theoretical reference for the defects nondestructive detection of hawthorn fruit.

Aiming for the complete utilization of sugar-beet pulp: Examination of the effects of mild acid and hydrothermal pretreatment followed by enzymatic digestion

PubMed Central

2011-01-01

Background Biomass use for the production of bioethanol or platform chemicals requires efficient breakdown of biomass to fermentable monosaccharides. Lignocellulosic feedstocks often require physicochemical pretreatment before enzymatic hydrolysis can begin. The optimal pretreatment can be different for different feedstocks, and should not lead to biomass destruction or formation of toxic products. Methods We examined the influence of six mild sulfuric acid or water pretreatments at different temperatures on the enzymatic degradability of sugar-beet pulp (SBP). Results We found that optimal pretreatment at 140°C of 15 minutes in water was able to solubilize 60% w/w of the total carbohydrates present, mainly pectins. More severe treatments led to the destruction of the solubilized sugars, and the subsequent production of the sugar-degradation products furfural, hydroxymethylfurfural, acetic acid and formic acid. The pretreated samples were successfully degraded enzymatically with an experimental cellulase preparation. Conclusions In this study, we found that pretreatment of SBP greatly facilitated the subsequent enzymatic degradation within economically feasible time ranges and enzyme levels. In addition, pretreatment of SBP can be useful to fractionate functional ingredients such as arabinans and pectins from cellulose. We found that the optimal combined severity factor to enhance the enzymatic degradation of SBP was between log R'0 = -2.0 and log R'0 = -1.5. The optimal pretreatment and enzyme treatment solubilized up to 80% of all sugars present in the SBP, including ≥90% of the cellulose. PMID:21627804

Comparison of Dilution, Filtration, and Microwave Digestion Sample Pretreatments in Elemental Profiling of Wine by ICP-MS.

PubMed

Godshaw, Joshua; Hopfer, Helene; Nelson, Jenny; Ebeler, Susan E

2017-09-25

Wine elemental composition varies by cultivar, geographic origin, viticultural and enological practices, and is often used for authenticity validation. Elemental analysis of wine by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging due to the potential for non-spectral interferences and plasma instability arising from organic matrix components. Sample preparation mitigates these interferences, however, conflicting recommendations of best practices in ICP-MS analysis of wine have been reported. This study compared direct dilution, microwave-assisted acid digestion, and two filtration sample pretreatments, acidification prior to filtration and filtration followed by acidification, in elemental profiling of one white and three red table wines by ICP-MS. Of 43 monitored isotopes, 37 varied by sample preparation method, with significantly higher results of 17 isotopes in the microwave-digested samples. Both filtration treatments resulted in lower results for 11 isotopes compared to the other methods. Finally, isotope dilution determination of copper based on natural abundances and the 63 Cu: 65 Cu instrument response ratio agreed with external calibration and confirmed a significant sample preparation effect. Overall, microwave digestion did not compare favorably, and direct dilution was found to provide the best compromise between ease of use and result accuracy and precision, although all preparation strategies were able to differentiate the wines.

Alcoholic extraction enables EPR analysis to characterize radiation-induced cellulosic signals in spices.

PubMed

Ahn, Jae-Jun; Sanyal, Bhaskar; Akram, Kashif; Kwon, Joong-Ho

2014-11-19

Different spices such as turmeric, oregano, and cinnamon were γ-irradiated at 1 and 10 kGy. The electron paramagnetic resonance (EPR) spectra of the nonirradiated samples were characterized by a single central signal (g = 2.006), the intensity of which was significantly enhanced upon irradiation. The EPR spectra of the irradiated spice samples were characterized by an additional triplet signal at g = 2.006 with a hyperfine coupling constant of 3 mT, associated with the cellulose radical. EPR analysis on various sample pretreatments in the irradiated spice samples demonstrated that the spectral features of the cellulose radical varied on the basis of the pretreatment protocol. Alcoholic extraction pretreatment produced considerable improvements of the EPR signals of the irradiated spice samples relative to the conventional oven and freeze-drying techniques. The alcoholic extraction process is therefore proposed as the most suitable sample pretreatment for unambiguous detection of irradiated spices by EPR spectroscopy.

Compositional and structural changes in Phoenix canariensis and Opuntia ficus-indica with pretreatment: Effects on enzymatic hydrolysis and second generation ethanol production.

PubMed

Udeh, Benard Anayo; Erkurt, Emrah Ahmet

2017-01-01

Two different plants namely Phoenix canariensis and Opuntia ficus-indica were used as substrate for reducing sugar generation and ethanol production. Dilute acid, alkaline and steam explosion were used as pretreatment methods in order to depolymerize lignin and/or hemicellulose and recover cellulose. By using alkaline pretreatment with 2.5% NaOH 71.08% for P. canariensis and 74.61% for O. ficus-indica lignin removal and 81.84% for P. canariensis and 72.66% for O. ficus-indica cellulose recovery yields were obtained. Pretreated materials were hydrolyzed by cellulase with high efficiency (87.0% and 84.5% cellulose conversion yields for P. canariensis and O. ficus-indica) and used as substrate for fermentation. Maximum ethanol production of 15.75g/L and 14.71g/L were achieved from P. canariensis and O. ficus-indica respectively. Structural differences were observed by XRD, FTIR and SEM for untreated, pretreated, hydrolyzed and fermented samples and were highly correlated with compositional analysis results. Copyright © 2016 Elsevier Ltd. All rights reserved.

Recent developments in sample preparation and data pre-treatment in metabonomics research.

PubMed

Li, Ning; Song, Yi peng; Tang, Huiru; Wang, Yulan

2016-01-01

Metabonomics is a powerful approach for biomarker discovery and an effective tool for pinpointing endpoint metabolic effects of external stimuli, such as pathogens and disease development. Due to its wide applications, metabonomics is required to deal with various biological samples of different properties. Hence sample preparation and corresponding data pre-treatment become important factors in ensuring validity of an investigation. In this review, we summarize some recent developments in metabonomics sample preparation and data-pretreatment procedures. Copyright © 2015 Elsevier Inc. All rights reserved.

Effect of postharvest pretreatments on organic Early Superior Seedless "Sugraone" table grapes assigned to long term storage

NASA Astrophysics Data System (ADS)

Admane, Naouel; Verrastro, Vincenzo; Di Gennaro, Domenico; Genovese, Francesco; Altieri, Giuseppe; Carlo Di Renzo, Giovanni

2014-05-01

Every year a significant amount of organic table grapes is lost during postharvest mainly due to the incidence of decay, stem browning and fast alteration of the taste and aroma. The demand for this fresh product with immaculate appearance and high sensory quality in terms of flavor, is a hard challenge considering the difficulties to conserve them, with alternative safe treatments to the sulphur dioxide (SO2) which is not allowed in organic product. The aim of this experiment was to maintain the quality of organic table grapes and extend their shelf-life for medium and long term, in order to reach new distant promising markets, by using safe methods. The effectiveness of the combination of pretreatment with Generally Recognized As Safe (GRAS) compounds, physical means and storage under modified atmosphere packaging (MAP) were performed by using detached organic table grape berries as alternatives to usual industrial SO2 application. The detached organic Early Superior Seedless "Sugraone" berries were pretreated by: i) dipping in ethanol and potassium bicarbonate; ii) massive CO2 concentrations; iii) ozone (O3) fumigation; whereas, untreated berries were included in the trial as control. Moreover, all the samples were packed in thermo-sealed ALPAK bags with MAP of 2% O2:5% CO2:93% N2 and stored at 0°C for 45 days. Initially and after 15, 30 and 45 days of storage, weight loss, decay incidence, berry/skin firmness, pedicel detachment force, skin color parameters, SSC, pH, titratable acidity and sensory evaluation scores, were monitored. After 45 days of storage, the weight loss was higher in the sample pretreated with massive CO2 concentration at 70 - 90 % and the control. The samples pretreated with CO2 at 70% and O3 at 20 ppm maintained the strength of the berry linked to its pedicel, also the berry and skin firmness were statistically higher in samples pretreated with CO2 at 90 - 70% and O3 at 20 ppm in comparison with the control. The skin color parameters and titratable acidity decreased, while, pH increased in all samples in comparison with their initial value. Also, the SSC increased in samples treated with O3 at 20 ppm, CO2 at 70% and dipping. Finally, the sensory evaluation scores gave the decisive data for the selection of the best combination treatments in order to validate their efficiency and that of the film packaging on late season organic table grape "Scarlotta/Sugraninteen". The highest scores for crunchiness, firmness, sweetness and sourness were given to samples pretreated by dipping. In conclusion, the efficiency of both film packaging and MAP inhibited the occurrence of berries decay in all samples including the control. These preliminary results represent the first step to design a treatment approach and develop a postharvest protocol for organic table grapes assigned to long term storage or shipping.

Flow-based analysis using microfluidics-chemiluminescence systems.

PubMed

Al Lawati, Haider A J

2013-01-01

This review will discuss various approaches and techniques in which analysis using microfluidics-chemiluminescence systems (MF-CL) has been reported. A variety of applications is examined, including environmental, pharmaceutical, biological, food and herbal analysis. Reported uses of CL reagents, sample introduction techniques, sample pretreatment methods, CL signal enhancement and detection systems are discussed. A hydrodynamic pumping system is predominately used for these applications. However, several reports are available in which electro-osmotic (EO) pumping has been implemented. Various sample pretreatment methods have been used, including liquid-liquid extraction, solid-phase extraction and molecularly imprinted polymers. A wide range of innovative techniques has been reported for CL signal enhancement. Most of these techniques are based on enhancement of the mixing process in the microfluidics channels, which leads to enhancement of the CL signal. However, other techniques are also reported, such as mirror reaction, liquid core waveguide, on-line pre-derivatization and the use of an opaque white chip with a thin transparent seal. Photodetectors are the most commonly used detectors; however, other detection systems have also been used, including integrated electrochemiluminescence (ECL) and organic photodiodes (OPDs). Copyright © 2012 John Wiley & Sons, Ltd.

Impact of contamination and pre-treatment on stable carbon and nitrogen isotopic composition of charred plant remains

PubMed Central

Vaiglova, Petra; Snoeck, Christophe; Nitsch, Erika; Bogaard, Amy; Lee-Thorp, Julia

2014-01-01

Rationale Stable isotope analysis of archaeological charred plants has become a useful tool for interpreting past agricultural practices and refining ancient dietary reconstruction. Charred material that lay buried in soil for millennia, however, is susceptible to various kinds of contamination, whose impact on the grain/seed isotopic composition is poorly understood. Pre-treatment protocols have been adapted in distinct forms from radiocarbon dating, but insufficient research has been carried out on evaluating their effectiveness and necessity for stable carbon and nitrogen isotope analysis. Methods The effects of previously used pre-treatment protocols on the isotopic composition of archaeological and modern sets of samples were investigated. An archaeological sample was also artificially contaminated with carbonates, nitrates and humic acid and subjected to treatment aimed at removing the introduced contamination. The presence and removal of the contamination were investigated using Fourier transform infrared spectroscopy (FTIR) and δ13C and δ15N values. Results The results show a ca 1‰ decrease in the δ15N values of archaeological charred plant material caused by harsh acid treatments and ultra-sonication. This change is interpreted as being caused by mechanical distortion of the grains/seeds rather than by the removal of contamination. Furthermore, specific infrared peaks have been identified that can be used to detect the three types of contaminants studied. We argue that it is not necessary to try to remove humic acid contamination for stable isotope analysis. The advantages and disadvantages of crushing the grains/seeds before pre-treatment are discussed. Conclusions We recommend the use of an acid-only procedure (0.5 M HCl for 30 min at 80°C followed by three rinses in distilled water) for cleaning charred plant remains. This study fills an important gap in plant stable isotope research that will enable future researchers to evaluate potential sources of isotopic change and pre-treat their samples with methods that have been demonstrated to be effective. © 2014 The Authors. Rapid Communications in Mass Spectrometry published by John Wiley & Sons Ltd. PMID:25366397

Variable selection based near infrared spectroscopy quantitative and qualitative analysis on wheat wet gluten

NASA Astrophysics Data System (ADS)

Lü, Chengxu; Jiang, Xunpeng; Zhou, Xingfan; Zhang, Yinqiao; Zhang, Naiqian; Wei, Chongfeng; Mao, Wenhua

2017-10-01

Wet gluten is a useful quality indicator for wheat, and short wave near infrared spectroscopy (NIRS) is a high performance technique with the advantage of economic rapid and nondestructive test. To study the feasibility of short wave NIRS analyzing wet gluten directly from wheat seed, 54 representative wheat seed samples were collected and scanned by spectrometer. 8 spectral pretreatment method and genetic algorithm (GA) variable selection method were used to optimize analysis. Both quantitative and qualitative model of wet gluten were built by partial least squares regression and discriminate analysis. For quantitative analysis, normalization is the optimized pretreatment method, 17 wet gluten sensitive variables are selected by GA, and GA model performs a better result than that of all variable model, with R2V=0.88, and RMSEV=1.47. For qualitative analysis, automatic weighted least squares baseline is the optimized pretreatment method, all variable models perform better results than those of GA models. The correct classification rates of 3 class of <24%, 24-30%, >30% wet gluten content are 95.45, 84.52, and 90.00%, respectively. The short wave NIRS technique shows potential for both quantitative and qualitative analysis of wet gluten for wheat seed.

Sensitive Voltammetric Determination of Natural Flavonoid Quercetin on a Disposable Graphite Lead

PubMed Central

Vu, Dai Long; Žabčíková, Simona; Ertek, Bensu; Dilgin, Yusuf

2015-01-01

Summary In this paper, a pencil graphite electrode was pretreated using chronoamperometry technique in phosphate buffer solution (pH=7.0) for sensitive determination of quercetin. Oxidation of quercetin was investigated using pretreated pencil graphite electrode and anodic stripping differential pulse voltammetry. Under optimal conditions, the anodic current of quercetin exhibited linear response to its concentration in the range from 0.001 to 1.5 µmol/L with the limit of detection of 0.3·10–3 µmol/L. The proposed method was successfully applied for the determination of quercetin in cranberry and blackcurrant juices with recovery rate from 93.2 to 94.7%. Solid-phase extraction was found to be necessary prior to voltammetric determination of quercetin in fruit juice samples using pretreated pencil graphite electrode. PMID:27904372

Surface and ultrastructural characterization of raw and pretreated switchgrass.

PubMed

Donohoe, Bryon S; Vinzant, Todd B; Elander, Richard T; Pallapolu, Venkata Ramesh; Lee, Y Y; Garlock, Rebecca J; Balan, Venkatesh; Dale, Bruce E; Kim, Youngmi; Mosier, Nathan S; Ladisch, Michael R; Falls, Matthew; Holtzapple, Mark T; Sierra-Ramirez, Rocio; Shi, Jian; Ebrik, Mirvat A; Redmond, Tim; Yang, Bin; Wyman, Charles E; Hames, Bonnie; Thomas, Steve; Warner, Ryan E

2011-12-01

The US Department of Energy-funded Biomass Refining CAFI (Consortium for Applied Fundamentals and Innovation) project has developed leading pretreatment technologies for application to switchgrass and has evaluated their effectiveness in recovering sugars from the coupled operations of pretreatment and enzymatic hydrolysis. Key chemical and physical characteristics have been determined for pretreated switchgrass samples. Several analytical microscopy approaches utilizing instruments in the Biomass Surface Characterization Laboratory (BSCL) at the National Renewable Energy Laboratory (NREL) have been applied to untreated and CAFI-pretreated switchgrass samples. The results of this work have shown that each of the CAFI pretreatment approaches on switchgrass result in different structural impacts at the plant tissue, cellular, and cell wall levels. Some of these structural changes can be related to changes in chemical composition upon pretreatment. There are also apparently different structural mechanisms that are responsible for achieving the highest enzymatic hydrolysis sugar yields. Copyright © 2011. Published by Elsevier Ltd.

Pretreatment HIV-drug resistance in Mexico and its impact on the effectiveness of first-line antiretroviral therapy: a nationally representative 2015 WHO survey.

PubMed

Ávila-Ríos, Santiago; García-Morales, Claudia; Matías-Florentino, Margarita; Romero-Mora, Karla A; Tapia-Trejo, Daniela; Quiroz-Morales, Verónica S; Reyes-Gopar, Helena; Ji, Hezhao; Sandstrom, Paul; Casillas-Rodríguez, Jesús; Sierra-Madero, Juan; León-Juárez, Eddie A; Valenzuela-Lara, Marisol; Magis-Rodríguez, Carlos; Uribe-Zuñiga, Patricia; Reyes-Terán, Gustavo

2016-12-01

WHO has developed a global HIV-drug resistance surveillance strategy, including assessment of pretreatment HIV-drug resistance. We aimed to do a nationally representative survey of pretreatment HIV-drug resistance in Mexico using WHO-recommended methods. Among 161 Ministry of Health antiretroviral therapy (ART) clinics in Mexico, the largest, including 90% of ART initiators within the Ministry of Health (66 in total), were eligible for the survey. We used a probability-proportional-to-size design method to sample 25 clinics throughout the country. Consecutive ART-naive patients with HIV about to initiate treatment were invited to participate in the survey; individuals with previous exposure to ART were excluded. We assessed pretreatment HIV-drug resistance by Sanger sequencing and next-generation sequencing of viruses from plasma specimens from eligible participants with Stanford University HIV Drug Resistance Database methods. We obtained follow-up data for a median of 9·4 months (range 6-12) after enrolment. We investigated possible relations between demographic variables and pretreatment drug resistance with univariate and multivariate logistic regression. Between Feb 3 and July 30, 2015, we screened 288 patients in 25 clinics, from whom 264 provided successfully sequenced viruses with no evidence of current exposure to antiretroviral drugs. With the Sanger method, of these 264 participants, 41 (15·5%, 95% CI 11·4-20·5) had pretreatment resistance to any antiretroviral drug and 28 (10·6%, 7·2-15·0) had pretreatment resistance to non-nucleoside reverse transcriptase inhibitors (NNRTIs). At least low-level pretreatment resistance (Stanford penalty score ≥15) was noted in 13 (4 · 9%) of participants to efavirenz and in 23 (8·7%) to the combination tenofovir plus emtricitabine plus efavirenz. With next-generation sequencing, of 264 participants, 38 (14·4%, 95% CI 10·4-19·2) had pretreatment resistance to any antiretroviral drug and 26 (9·8%, 6·5-14·1) had pretreatment resistance to NNRTIs. After median follow-up of 8 months (IQR 6·5-9·4, range 5-11) after ART initiation, 97 (72%) of 135 NNRTI initiators achieved viral suppression (<50 copies per mL) compared with ten (40%) of 25 individuals who started with protease inhibitor-based regimens (p=0·0045). After multivariate regression considering pretreatment resistance and initial ART regimen as composite variables, people starting NNRTIs with pretreatment drug resistance achieved significantly lower viral suppression (odds ratio 0·24, 95% CI 0·07-0·74; p=0·014) than patients without NNRTI resistance. High levels of pretreatment drug resistance were noted in Mexico, and NNRTI pretreatment drug resistance significantly reduced the effectiveness of first-line ART regimens based on these drugs. Baseline HIV-drug resistance testing for initial ART follow-up and decision making should be considered. The Mexican Government and Consejo Nacional de Ciencia y Tecnología. Copyright © 2016 Elsevier Ltd. All rights reserved.

Improving the sludge disintegration efficiency of sonication by combining with alkalization and thermal pre-treatment methods.

PubMed

Şahinkaya, S; Sevimli, M F; Aygün, A

2012-01-01

One of the most serious problems encountered in biological wastewater treatment processes is the production of waste activated sludge (WAS). Sonication, which is an energy-intensive process, is the most powerful sludge pre-treatment method. Due to lack of information about the combined pre-treatment methods of sonication, the combined pre-treatment methods were investigated and it was aimed to improve the disintegration efficiency of sonication by combining sonication with alkalization and thermal pre-treatment methods in this study. The process performances were evaluated based on the quantities of increases in soluble chemical oxygen demand (COD), protein and carbohydrate. The releases of soluble COD, carbohydrate and protein by the combined methods were higher than those by sonication, alkalization and thermal pre-treatment alone. Degrees of sludge disintegration in various options of sonication were in the following descending order: sono-alkalization > sono-thermal pre-treatment > sonication. Therefore, it was determined that combining sonication with alkalization significantly improved the sludge disintegration and decreased the required energy to reach the same yield by sonication. In addition, effects on sludge settleability and dewaterability and kinetic mathematical modelling of pre-treatment performances of these methods were investigated. It was proven that the proposed model accurately predicted the efficiencies of ultrasonic pre-treatment methods.

Voltammetric Electronic Tongue and Support Vector Machines for Identification of Selected Features in Mexican Coffee

PubMed Central

Domínguez, Rocio Berenice; Moreno-Barón, Laura; Muñoz, Roberto; Gutiérrez, Juan Manuel

2014-01-01

This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure. PMID:25254303

Voltammetric electronic tongue and support vector machines for identification of selected features in Mexican coffee.

PubMed

Domínguez, Rocio Berenice; Moreno-Barón, Laura; Muñoz, Roberto; Gutiérrez, Juan Manuel

2014-09-24

This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure.

Extraction Methods in Soil Phosphorus Characterisation

NASA Astrophysics Data System (ADS)

Soinne, Helena

2010-05-01

Extraction methods are widely used to assess the bioavailability of P and to characterise soil P reserves. Even though new and more sophisticated methods to characterise soil P are constantly developed the use of extraction methods is not likely to be replaced because of the relatively simple analytical equipment needed for the analysis. However, the large variety of extractants, pre-treatments and sample preparation procedures complicate the comparison of published results. In order to improve our understanding of the behaviour and cycling of P in soil, it is important to know the role of extracted P in the soil P cycle. The knowledge of the factors affecting the analytical outcome is a prerequisite for justified interpretation of the results. In this study, the effect of sample pre-treatment and properties of the used extractant on extractable molybdate-reactive phosphorus (MRP) and molybdate-unreactive phosphorus (MUP) was studied. Furthermore, the effect of sample preparation procedures prior the analysis on measured MRP and MUP was studied. Two widely used sequential extraction procedures were compared on their ability to show management induced differences on soil P. These results revealed that pre-treatments changed soil properties and air-drying was found to affect soil P, particularly extractable MUP, thought to represent organic P, by disrupting organic matter. This was evidenced by an increase in the water-extractable small-sized (<0.2 µm) P that, at least partly, took place at the expense of the large-sized (>0.2 µm) P. In addition to the effects of sample pre-treatment, the results showed that extractable organic P was sensitive to the chemical nature of the used extractant and to the sample preparation procedures employed prior to P analysis, including centrifugation and filtering of soil suspensions. Filtering may remove a major proportion of extractable MUP; therefore filtering cannot be recommended in the characterisation of solubilised MUP. However, extractants having high ionic strength may cause the organic molecules to collapse during centrifugation and thus affect the recovered concentration of MUP. These findings highlight the importance of characterising the nature of the MUP extracted with different extractants and acknowledging the sensitivity of MUP to analytical procedures when comparing published results. Widely used sequential fractionation procedures proved to be able to detect land-use -derived differences in the distribution of P among fractions of different solubilities. The results of this study demonstrate that, although the extraction methods do not reveal the biogeochemical function of a given P pool in soil, the extraction methods can be used to detect changes in soil P pools with different solubilities. To obtain the most benefit from extraction methods, we need a better understanding of the biological availability of P and the role of extracted P fraction in the P cycle in soils from different environments (climatic and weather) and land-uses.

Influence of physicochemical treatments on iron-based spent catalyst for catalytic oxidation of toluene.

PubMed

Kim, Sang Chai; Shim, Wang Geun

2008-06-15

The catalytic oxidation of toluene was studied over an iron-based spent and regenerated catalysts. Air, hydrogen, or four different acid solutions (oxalic acid (C2H2O4), citric acid (C6H8O7), acetic acid (CH3COOH), and nitric acid (HNO3)) were employed to regenerate the spent catalyst. The properties of pretreated spent catalyst were characterized by the Brunauer Emmett Teller (BET), inductively coupled plasma (ICP), temperature programmed reduction (TPR), and X-ray diffraction (XRD) analyses. The air pretreatment significantly enhanced the catalytic activity of the spent catalyst in the pretreatment temperature range of 200-400 degrees C, but its catalytic activity diminished at the pretreatment temperature of 600 degrees C. The catalytic activity sequence with respect to the air pretreatment temperatures was 400 degrees C>200 degrees C>parent>600 degrees C. The TPR results indicated that the catalytic activity was correlated with both the oxygen mobility and the amount of available oxygen on the catalyst. In contrast, the hydrogen pretreatment had a negative effect on the catalytic activity, and toluene conversion decreased with increasing pretreatment temperatures (200-600 degrees C). The XRD and TPR results confirmed the formation of metallic iron which had a negative effect on the catalytic activity with increasing pretreatment temperature. The acid pretreatment improved the catalytic activity of the spent catalyst. The catalytic activity sequence with respect to different acids pretreatment was found to be oxalic acid>citric acid>acetic acid>or=nitric acid>parent. The TPR results of acid pretreated samples showed an increased amount of available oxygen which gave a positive effect on the catalytic activity. Accordingly, air or acid pretreatments were more promising methods of regenerating the iron-based spent catalyst. In particular, the oxalic acid pretreatment was found to be most effective in the formation of FeC2O4 species which contributed highly to the catalytic combustion of toluene.

Combined alkaline and ultrasonic pretreatment of sludge before aerobic digestion.

PubMed

Jin, Yiying; Li, Huan; Mahar, Rasool Bux; Wang, Zhiyu; Nie, Yongfeng

2009-01-01

Alkaline and ultrasonic sludge disintegration can be used as the pretreatment of waste activated sludge (WAS) to promote the subsequent anaerobic or aerobic digestion. In this study, different combinations of these two methods were investigated. The evaluation was based on the quantity of soluble chemical oxygen demand (SCOD) in the pretreated sludge as well as the degradation of organic matter in the subsequent aerobic digestion. For WAS samples with combined pretreatment, the released COD levels were higher than those with ultrasonic or alkaline pretreatment alone. When combined with the ultrasonic treatment, NaOH treatment was more efficient than Ca(OH)2 for WAS solubilization. The COD levels released in various sequential options of combined NaOH and ultrasonic treatments were in the the following descending order: simultaneous treatment > NaOH treatment followed by ultrasonic treatment > ultrasonic treatment followed by NaOH treatment. For simultaneous treatment, low NaOH dosage (100 g/kg dry solid), short duration (30 min) of NaOH treatment, and low ultrasonic specific energy (7500 kJ/kg dry solid) were suitable for sludge disintegration. Using combined NaOH and ultrasonic pretreatment with optimal parameters, the degradation efficiency of organic matter was increased from 38.0% to 50.7%, which is much higher than that with ultrasonic (42.5%) or with NaOH pretreatment (43.5%) in the subsequent aerobic digestion at the same retention time.

Prognostic significance of the lymphocyte-to-monocyte ratio in patients with metastatic colorectal cancer

PubMed Central

Shibutani, Masatsune; Maeda, Kiyoshi; Nagahara, Hisashi; Ohtani, Hiroshi; Sakurai, Katsunobu; Yamazoe, Sadaaki; Kimura, Kenjiro; Toyokawa, Takahiro; Amano, Ryosuke; Tanaka, Hiroaki; Muguruma, Kazuya; Hirakawa, Kosei

2015-01-01

AIM: To evaluate the prognostic significance of the lymphocyte to monocyte ratio (LMR) in patients with unresectable metastatic colorectal cancer who received palliative chemotherapy. METHODS: A total of 104 patients with unresectable metastatic colorectal cancer who underwent palliative chemotherapy were enrolled. The LMR was calculated from blood samples by dividing the absolute lymphocyte count by the absolute monocyte count. Pre-treatment LMR values were measured within one week before the initiation of chemotherapy, while post-treatment LMR values were measured eight weeks after the initiation of chemotherapy. RESULTS: The median pre-treatment LMR was 4.16 (range: 0.58-14.06). We set 3.38 as the cut-off level based on the receiver operating characteristic curve. Based on the cut-off level of 3.38, 66 patients were classified into the high pre-treatment LMR group and 38 patients were classified into the low pre-treatment LMR group. The low pre-treatment LMR group had a significantly worse overall survival rate (P = 0.0011). Moreover, patients who demonstrated low pre-treatment LMR and normalization after treatment exhibited a better overall survival rate than the patients with low pre-treatment and post-treatment LMR values. CONCLUSION: The lymphocyte to monocyte ratio is a useful prognostic marker in patients with unresectable metastatic colorectal cancer who receive palliative chemotherapy. PMID:26379401

Enhancement of enzymatic saccharification of Eucalyptus globulus: steam explosion versus steam treatment.

PubMed

Martin-Sampedro, Raquel; Revilla, Esteban; Villar, Juan C; Eugenio, Maria E

2014-09-01

Steam explosion and steam pre-treatment have proved capable of enhancing enzymatic saccharification of lignocellulosic materials. However, until now, these methods had not been compared under the same operational conditions and using the same raw material. Both pre-treatments lead to increased yields in the saccharification of Eucalyptus globulus; but results have been better with steam pre-treatments, despite the more accessible surface of exploded samples. The reason for this finding could be enzymatic inhibition: steam explosion causes a more extensive extraction of hemicelluloses and releases a greater amount of degradation products which can inhibit enzymatic action. Enzymatic inhibition is also dependent on the amount and chemical structure of lignin, which was also a contributing factor to the lower enzymatic yields obtained with the most severe pre-treatment. Thus, the highest yields (46.7% glucose and 73.4% xylose yields) were obtained after two cycle of steam treatment, of 5 and 3 min, at 183°C. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of ultrasound pre-treatment on the drying kinetics of brown seaweed Ascophyllum nodosum.

PubMed

Kadam, Shekhar U; Tiwari, Brijesh K; O'Donnell, Colm P

2015-03-01

The effect of ultrasound pre-treatment on the drying kinetics of brown seaweed Ascophyllum nodosum under hot-air convective drying was investigated. Pretreatments were carried out at ultrasound intensity levels ranging from 7.00 to 75.78 Wcm(-2) for 10 min using an ultrasonic probe system. It was observed that ultrasound pre-treatments reduced the drying time required. The shortest drying times were obtained from samples pre-treated at 75.78 Wcm(-2). The fit quality of 6 thin-layer drying models was also evaluated using the determination of coefficient (R(2)), root means square error (RMSE), AIC (Akaike information criterion) and BIC (Bayesian information criterion). Drying kinetics were modelled using the Newton, Henderson and Pabis, Page, Wang and Singh, Midilli et al. and Weibull models. The Newton, Wang and Singh, and Midilli et al. models showed the best fit to the experimental drying data. Color of ultrasound pretreated dried seaweed samples were lighter compared to control samples. It was concluded that ultrasound pretreatment can be effectively used to reduce the energy cost and drying time for drying of A. nodosum. Copyright © 2014 Elsevier B.V. All rights reserved.

Standardization and optimization of fluorescence in situ hybridization (FISH) for HER-2 assessment in breast cancer: A single center experience.

PubMed

Bogdanovska-Todorovska, Magdalena; Petrushevska, Gordana; Janevska, Vesna; Spasevska, Liljana; Kostadinova-Kunovska, Slavica

2018-05-20

Accurate assessment of human epidermal growth factor receptor 2 (HER-2) is crucial in selecting patients for targeted therapy. Commonly used methods for HER-2 testing are immunohistochemistry (IHC) and fluorescence in situ hybridization (FISH). Here we presented the implementation, optimization and standardization of two FISH protocols using breast cancer samples and assessed the impact of pre-analytical and analytical factors on HER-2 testing. Formalin fixed paraffin embedded (FFPE) tissue samples from 70 breast cancer patients were tested for HER-2 using PathVysion™ HER-2 DNA Probe Kit and two different paraffin pretreatment kits, Vysis/Abbott Paraffin Pretreatment Reagent Kit (40 samples) and DAKO Histology FISH Accessory Kit (30 samples). The concordance between FISH and IHC results was determined. Pre-analytical and analytical factors (i.e., fixation, baking, digestion, and post-hybridization washing) affected the efficiency and quality of hybridization. The overall hybridization success in our study was 98.6% (69/70); the failure rate was 1.4%. The DAKO pretreatment kit was more time-efficient and resulted in more uniform signals that were easier to interpret, compared to the Vysis/Abbott kit. The overall concordance between IHC and FISH was 84.06%, kappa coefficient 0.5976 (p < 0.0001). The greatest discordance (82%) between IHC and FISH was observed in IHC 2+ group. A standardized FISH protocol for HER-2 assessment, with high hybridization efficiency, is necessary due to variability in tissue processing and individual tissue characteristics. Differences in the pre-analytical and analytical steps can affect the hybridization quality and efficiency. The use of DAKO pretreatment kit is time-saving and cost-effective.

Determination of proflavine in rat whole blood without sample pretreatment by laser desorption postionization mass spectrometry.

PubMed

Chen, Jiaxin; Hu, Yongjun; Lu, Qiao; Wang, Pengchao; Zhan, Huaqi

2017-04-01

A novel pretreatment-free method involving laser desorption postionization (LDPI) coupled with time-of-flight mass spectrometry (MS) was developed for the monitoring of proflavine level in rat whole blood. It comprises a protocol for dosing via intravenous administration and collection of whole blood, followed by direct LDPI-MS analysis without any sample pretreatment. An intense ion signal at m/z 209 was observed from whole blood without any interference signals, except some background signals below m/z 100. The calibration curve was established with use of 9-phenylacridine as the internal standard for proflavine determination from the plotting of the peak ratios of proflavine to the internal standard, with a correlation coefficient (R 2 ) greater than 0.99. The limit of detection was estimated to be 0.48 pmol/mm 2 and the quantification range was 0.5-16.5 μg/mL for proflavine. In addition, only a minimal matrix effect was observed, as expected from considerations of the desorption and ionization mechanism. Interday and intraday accuracy and precision were calculated to be within 13% and 82-114%, respectively. Estimated concentrations of proflavine residue in whole blood were also successfully obtained at selected time points after dosing. The proposed method is simple, low cost, and sensitive, and should be seen as a complementary method for monitoring drug levels in blood. Graphical Abstract Monitoring proflavine levels in rat whole blood at different time points using laser desorption postionization mass spectrometry (LDPI-MS).

Topochemical Analysis of Cell Wall Components by TOF-SIMS.

PubMed

Aoki, Dan; Fukushima, Kazuhiko

2017-01-01

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a recently developing analytical tool and a type of imaging mass spectrometry. TOF-SIMS provides mass spectral information with a lateral resolution on the order of submicrons, with widespread applicability. Sometimes, it is described as a surface analysis method without the requirement for sample pretreatment; however, several points need to be taken into account for the complete utilization of the capabilities of TOF-SIMS. In this chapter, we introduce methods for TOF-SIMS sample treatments, as well as basic knowledge of wood samples TOF-SIMS spectral and image data analysis.

Experimental study and neural network modeling of sugarcane bagasse pretreatment with H2SO4 and O3 for cellulosic material conversion to sugar.

PubMed

Gitifar, Vahid; Eslamloueyan, Reza; Sarshar, Mohammad

2013-11-01

In this study, pretreatment of sugarcane bagasse and subsequent enzymatic hydrolysis is investigated using two categories of pretreatment methods: dilute acid (DA) pretreatment and combined DA-ozonolysis (DAO) method. Both methods are accomplished at different solid ratios, sulfuric acid concentrations, autoclave residence times, bagasse moisture content, and ozonolysis time. The results show that the DAO pretreatment can significantly increase the production of glucose compared to DA method. Applying k-fold cross validation method, two optimal artificial neural networks (ANNs) are trained for estimations of glucose concentrations for DA and DAO pretreatment methods. Comparing the modeling results with experimental data indicates that the proposed ANNs have good estimation abilities. Copyright © 2013 Elsevier Ltd. All rights reserved.

Comparative evaluation of acid and alkaline sulfite pretreatments for enzymatic saccharification of bagasses from three different sugarcane hybrids.

PubMed

Monte, Joseana R; Laurito-Friend, Debora F; Ferraz, André; Milagres, Adriane M F

2018-04-26

Sugarcane bagasses from three experimental sugarcane hybrids and a mill-reference sample were used to compare the efficiency and mode of action of acid and alkaline sulfite pretreatment processes. Varied chemical loads and reaction temperatures were used to prepare samples with distinguished characteristics regarding xylan and lignin removals, as well as sulfonation levels of residual lignins. The pretreatment with low sulfite loads (5%) under acidic conditions (pH 2) provided maximum glucose yield of 70% during enzymatic hydrolysis with cellulases (10 FPU/g) and β-glucosidases (20 UI/g bagasse). In this case, glucan enzymatic conversion from pretreated materials was mostly associated with extensive xylan removal (70-100%) and partial delignification occurred during the pretreatment. The use of low sulfite loads under acidic conditions required pretreatment temperatures of 160°C. In contrast, at a lower pretreatment temperature (120°C), alkaline sulfite process achieved similar glucan digestibility, but required a higher sulfite load (7.5%). Residual xylans from acid pretreated materials were almost completely hydrolysed by commercial enzymes, contrasting with relatively lower xylan to xylose conversions observed in alkaline pretreated samples. Efficient xylan removal during acid sulfite pretreatment and also during enzymatic digestion can be useful to enhance glucan accessibility and digestibility by cellulases. Alkaline sulfite process also provided substrates with high glucan digestibility, mainly associated with delignification and sulfonation of residual lignins. The results demonstrate that temperature, pH and sulfite can be combined for reducing lignocellulose recalcitrance and achieve similar glucan conversion rates in the alkaline and acid sulfite pretreated bagasses. This article is protected by copyright. All rights reserved. © 2018 American Institute of Chemical Engineers.

Methods for producing extracted and digested products from pretreated lignocellulosic biomass

DOEpatents

Chundawat, Shishir; Sousa, Leonardo Da Costa; Cheh, Albert M.; Balan; , Venkatesh; Dale, Bruce

2017-05-16

Methods for producing extracted and digested products from pretreated lignocellulosic biomass are provided. The methods include converting native cellulose I.sub..beta. to cellulose III.sub.I by pretreating the lignocellulosic biomass with liquid ammonia under certain conditions, and performing extracting or digesting steps on the pretreated/converted lignocellulosic biomass.

Effect of enzymatic pretreatment on the physical quality of plantain (Musa ssp., group AAB) employing airflow reversal drying.

PubMed

Rodríguez-Miranda, J; Martínez-Sánchez, C E; Hernández-Santos, B; Juárez-Barrientos, J M; Ventura-Báez, E G; Herman-Lara, E

2018-01-01

This work aimed to evaluate the effect of enzymatic pretreatment on the color and texture of plantain ( Musa ssp., group AAB) dried by airflow reversal drying. Plantain slices 1.0 cm thick were used. Pretreatment with two commercial enzymes, Pectinex Ultra SPL ( Aspergillus aculeatus ) and Pectinex 3XL ( Aspergillus niger ), was performed. Drying kinetics were determined with and without pretreatment at temperatures of 50, 65 and 80 °C using a fixed bed convective dryer. An air speed of 6 m/s, a bed height of 5 cm and either unidirectional flow or airflow reversal (every 15 min) were used for drying. Color and texture were analyzed, and consumer acceptance of the results of the best treatments was determined. Pretreatment with the enzyme A. niger and airflow reversal gave the best drying kinetics and showed the greatest reduction in drying time (59.0%) at 80 °C. The best hardness results were found at 80 °C with A. niger enzymatic pretreatment with both types of air flow. Brightness and hue angle showed that samples pretreated with enzymes and dried at 65 °C had a lighter yellow color compared to non-pretreated samples. Plantain samples enzymatically pretreated and dried at 65 and 80 °C were the most accepted by consumers. This kind of enzymatic pretreatment on plantain could allow the conservation of some physical properties and reduction of drying times relative to the current methodology.

Fabrication of Flower-like ZnO Micro/Nanostructures for Photodegradation of Pre-treated Palm Oil Mill Effluent

NASA Astrophysics Data System (ADS)

Lam, Sze-Mun; Wong, Kok-Ann; Sin, Jin-Chung

2018-01-01

Flower-like ZnO micro/nanostructures were fabricated by a simple and surfactant-free reflux method. X-ray diffraction findings showed that the prepared ZnO product was highly crystallite with hexagonal wurtzite structure. The band gap energy of ZnO sample was measured to be 3.18 eV via an optical reflectance spectrum. The flower-like morphological features of ZnO micro/nanostructures were witnessed through field-emission scanning electron microscopy. Such micro/nanoparticles could be used in the photodegradation of pre-treated palm oil mil effluent (POME) under UV irradiation.

Quality Characteristics and Quantification of Acetaldehyde and Methanol in Apple Wine Fermentation by Various Pre-Treatments of Mash

PubMed Central

Won, Seon Yi; Seo, Jae Soon; Kwak, Han Sub; Lee, Youngseung; Kim, Misook; Shim, Hyoung-Seok; Jeong, Yoonhwa

2015-01-01

The objective of this study was to compare the effects of adding lactic acid and pectinase, and chaptalization for the quality of apple wine and the production of hazardous compounds (methanol and acetaldehyde). The pH of all of the samples was below 4; therefore, mash seemed to be fermented without any issue. Total acidity was the highest in sample A due to lactic acid addition. Pre-treated groups (samples B, C, and D) showed higher total acidities than that of the control (P<0.05). Pre-treatments might influence the production of organic acids in apple wines. The control and pectinase added sample (sample B) had the lowest alcohol contents. Adding lactic acid produced more alcohol, and chaptalized samples produced more alcohol due to the addition of sugar. Adding pectinase with and without chaptalization was not effective for producing more alcohol. The control sample had significantly higher acetaldehyde content (2.39 mg/L) than the other samples (1.00~2.07 mg/L); therefore, pre-treatments for apple wine fermentation produced a lower amount of acetaldehyde. Among the pre-treated samples, samples C and D showed the lowest acetaldehyde content of 1.00 mg/L and 1.16 mg/L, respectively. On the other hand, a significantly higher amount of methanol was generated for sample A (1.03 mg/L) and sample D (1.22 mg/L) than that of the control (0.82 mg/L) (P<0.05). Adding lactic acid or chaptalization was effective in reducing methanol and acetaldehyde in apple wines. PMID:26770917

Toxoplasma Gondii and Pre-treatment Protocols for Polymerase Chain Reaction Analysis of Milk Samples: A Field Trial in Sheep from Southern Italy.

PubMed

Vismarra, Alice; Barilli, Elena; Miceli, Maura; Mangia, Carlo; Bacci, Cristina; Brindani, Franco; Kramer, Laura

2017-01-24

Toxoplasmosis is a zoonotic disease caused by the protozoan Toxoplasma gondii. Ingestion of raw milk has been suggested as a risk for transmission to humans. Here the authors evaluated pre-treatment protocols for DNA extraction on T. gondii tachyzoite-spiked sheep milk with the aim of identifying the method that resulted in the most rapid and reliable polymerase chain reaction (PCR) positivity. This protocol was then used to analyse milk samples from sheep of three different farms in Southern Italy, including real time PCR for DNA quantification and PCR-restriction fragment length polymorphism for genotyping. The pre-treatment protocol using ethylenediaminetetraacetic acid and Tris-HCl to remove casein gave the best results in the least amount of time compared to the others on spiked milk samples. One sample of 21 collected from sheep farms was positive on one-step PCR, real time PCR and resulted in a Type I genotype at one locus (SAG3). Milk usually contains a low number of tachyzoites and this could be a limiting factor for molecular identification. Our preliminary data has evaluated a rapid, cost-effective and sensitive protocol to treat milk before DNA extraction. The results of the present study also confirm the possibility of T. gondii transmission through consumption of raw milk and its unpasteurised derivatives.

Surface modification of polypropylene based particle foams

NASA Astrophysics Data System (ADS)

Schreier, P.; Trassl, C.; Altstädt, V.

2014-05-01

This paper deals with the modification of the surface properties of expanded polypropylene (EPP). EPP is a semi-hard to soft elastic thermoplastic foam. The characteristic surface of EPP shows process-related steam nozzle imprints and gussets. Therefore EPP does not satisfy the quality requirements for visible automotive applications. In order to meet these demands, plastic surfaces are usually enhanced with functional or decorative coatings, e.g. textiles, plastic films or paint. The coating of plastics with low surface energies such as PP often leads to adhesion problems by reason of the missing polar and functional groups. This paper gives an evaluation of activation and pre-treatment methods of EPP, with the aim to identify the most suitable pre-treatment method. For this purpose five typical surface treatment methods - flame treatment, corona, fluorination, atmospheric and low-pressure plasma - were performed on EPP samples. As a comparison criterion the maximum increase in the adhesion force between a polyurethane-based coating and the modified EPP substrate was selected. Moreover the influence of the selected pre-treatment method on the increase in the total surface energy and its polar component was investigated by the drop shape analysis method. The results showed that the contact angle measurement is a suitable method to determine the polar and disperse fractions of the surface tension of EPP. Furthermore, all performed methods increased the adhesion of EPP.

A statistical analysis of the effects of urease pre-treatment on the measurement of the urinary metabolome by gas chromatography–mass spectrometry

DOE PAGES

Webb-Robertson, Bobbie-Jo; Kim, Young -Mo; Zink, Erika M.; ...

2014-02-27

Urease pre-treatment of urine has been utilized since the early 1960s to remove high levels of urea from samples prior to further processing and analysis by gas chromatography-mass spectrometry (GC-MS). Aside from the obvious depletion or elimination of urea, the effect, if any, of urease pre-treatment on the urinary metabolome has not been studied in detail. Here, we report the results of three separate but related experiments that were designed to assess possible indirect effects of urease pre-treatment on the urinary metabolome as measured by GC-MS. In total, 235 GC-MS analyses were performed and over 106 identified and 200 unidentifiedmore » metabolites were quantified across the three experiments. The results showed that data from urease pre-treated samples 1) had the same or lower coefficients of variance among reproducibly detected metabolites, 2) more accurately reflected quantitative differences and the expected ratios among different urine volumes, and 3) increased the number of metabolite identifications. Altogether, we observed no negative consequences of urease pre-treatment. In contrast, urease pretreatment enhanced the ability to distinguish between volume-based and biological sample types compared to no treatment. Taken together, these results show that urease pretreatment of urine offers multiple beneficial effects that outweigh any artifacts that may be introduced to the data in urinary metabolomics analyses.« less

A Statistical Analysis of the Effects of Urease Pre-treatment on the Measurement of the Urinary Metabolome by Gas Chromatography-Mass Spectrometry

PubMed Central

Webb-Robertson, Bobbie-Jo; Kim, Young-Mo; Zink, Erika M.; Hallaian, Katherine A.; Zhang, Qibin; Madupu, Ramana; Waters, Katrina M.; Metz, Thomas O.

2014-01-01

Urease pre-treatment of urine has been utilized since the early 1960s to remove high levels of urea from samples prior to further processing and analysis by gas chromatography-mass spectrometry (GC-MS). Aside from the obvious depletion or elimination of urea, the effect, if any, of urease pre-treatment on the urinary metabolome has not been studied in detail. Here, we report the results of three separate but related experiments that were designed to assess possible indirect effects of urease pre-treatment on the urinary metabolome as measured by GC-MS. In total, 235 GC-MS analyses were performed and over 106 identified and 200 unidentified metabolites were quantified across the three experiments. The results showed that data from urease pre-treated samples 1) had the same or lower coefficients of variance among reproducibly detected metabolites, 2) more accurately reflected quantitative differences and the expected ratios among different urine volumes, and 3) increased the number of metabolite identifications. Overall, we observed no negative consequences of urease pre-treatment. In contrast, urease pretreatment enhanced the ability to distinguish between volume-based and biological sample types compared to no treatment. Taken together, these results show that urease pretreatment of urine offers multiple beneficial effects that outweigh any artifacts that may be introduced to the data in urinary metabolomics analyses. PMID:25254001

Effect of various pretreatment methods on anaerobic mixed microflora to enhance biohydrogen production utilizing dairy wastewater as substrate.

PubMed

Venkata Mohan, S; Lalit Babu, V; Sarma, P N

2008-01-01

Influence of different pretreatment methods applied on anaerobic mixed inoculum was evaluated for selectively enriching the hydrogen (H(2)) producing mixed culture using dairy wastewater as substrate. The experimental data showed the feasibility of molecular biohydrogen generation utilizing dairy wastewater as primary carbon source through metabolic participation. However, the efficiency of H(2) evolution and substrate removal efficiency were found to be dependent on the type of pretreatment procedure adopted on the parent inoculum. Among the studied pretreatment methods, chemical pretreatment (2-bromoethane sulphonic acid sodium salt (0.2 g/l); 24 h) procedure enabled higher H(2) yield along with concurrent substrate removal efficiency. On the contrary, heat-shock pretreatment (100 degrees C; 1 h) procedure resulted in relatively low H(2) yield. Compared to control experiments all the adopted pretreatment methods documented higher H(2) generation efficiency. In the case of combination experiments, integration of pH (pH 3; adjusted with ortho-phosphoric acid; 24 h) and chemical pretreatment evidenced higher H(2) production. Data envelopment analysis (DEA), a frontier analysis technique model was successfully applied to enumerate the relative efficiency of different pretreatment methods studied by considered pretreatment procedures as input and cumulative H(2) production rate and substrate degradation rate as corresponding two outputs.

Comparison of different pretreatment methods for separation hemicellulose from straw during the lignocellulosic bioethanol production

NASA Astrophysics Data System (ADS)

Eisenhuber, Katharina; Krennhuber, Klaus; Steinmüller, Viktoria; Kahr, Heike; Jäger, Alexander

2013-04-01

The combustion of fossil fuels is responsible for 73% of carbon dioxide emissions into the atmosphere and consequently contributes to global warming. This fact has enormously increased the interest in the development of methods to reduce greenhouse gases. Therefore, the focus is on the production of biofuels from lignocellulosic agricultural residues. The feedstocks used for 2nd generation bioethanol production are lignocellulosic raw materials like different straw types or energy crops like miscanthus sinensis or arundo donax. Lignocellulose consists of hemicellulose (xylose and arabinose), which is bonded to cellulose (glucose) and lignin. Prior to an enzymatic hydrolysis of the polysaccharides and fermentation of the resulting sugars, the lignocelluloses must be pretreated to make the sugar polymers accessible to enzymes. A variety of pretreatment methods are described in the literature: thermophysical, acid-based and alkaline methods.In this study, we examined and compared the most important pretreatment methods: Steam explosion versus acid and alkaline pretreatment. Specific attention was paid to the mass balance, the recovery of C 5 sugars and consumption of chemicals needed for pretreatment. In lab scale experiments, wheat straw was either directly pretreated by steam explosion or by two different protocols. The straw was either soaked in sulfuric acid or in sodium hydroxide solution at different concentrations. For both methods, wheat straw was pretreated at 100°C for 30 minutes. Afterwards, the remaining straw was separated by vacuum filtration from the liquid fraction.The pretreated straw was neutralized, dried and enzymatically hydrolyzed. Finally, the sugar concentrations (glucose, xylose and arabinose) from filtrate and from hydrolysate were determined by HPLC. The recovery of xylose from hemicellulose was about 50% using the sulfuric acid pretreatment and less than 2% using the sodium hydroxide pretreatment. Increasing concentrations of sulfuric acid lead to increasing conversion of hemicellulose to xylose. In contrast, increasing sodium hydroxide concentrations degrade the hemicellulose to unknown derivates. Consequently, almost no sugars from hemicellulose remain for fermentation. The hydrolysis of sulfuric acid pretreated straw results in a maximum glucose concentration of 100 g/kg straw and a xylose concentration of nearly 30 g/kg. Sodium hydroxide pretreated and hydrolyzed straw leads to a maximum glucose concentration of 90 g/kg straw and a xylose concentration of nearly 20 g/kg. In comparison to the two chemical pretreatment methods (sodium hydroxide and sulfuric acid pretreatment), the steam explosion pretreatment (conditions: temperature 190°C, time 20 minutes) results in a higher glucose concentration of about 190 g/kg straw and a xylose concentration of nearly 75 g/kg straw after enzymatic hydrolysis of the dried straw. Because of the small effect the sodium hydroxide pretreatment has on xylose recovery, this method won't be used for separation and conversion of hemicellulose into xylose and arabinose. Although pretreatment with sulfuric acid achieved promising results, further research and economical considerations have to be performed. In conclusion, the steam explosion method is still the state of the art pretreatment method for the production of lignocellulosic biofuels. Alkaline methods destroy most of the xylose part of the sugar fraction and a loss of up to 25 % of the fermentable sugars is not acceptable for a sustainable biofuel production. The acid pretreatment yields high amounts of accessible hemicellulose and cellulose, but the consumption of chemicals for acid pretreatment and neutralization has to be taken into account when considering technical implementation.

Negative interference by rheumatoid factor in alpha-fetoprotein chemiluminescent microparticle immunoassay.

PubMed

Wang, Hui; Bi, Xiaohui; Xu, Lei; Li, Yirong

2017-01-01

Background Rheumatoid factor causes positive interference in multiple immunoassays. Recently, negative interference has also been found in immunoassays in the presence of rheumatoid factor. The chemiluminescent microparticle immunoassay is widely used to determine serum alpha-fetoprotein. However, it is not clear whether the presence of rheumatoid factor in the serum causes interference in the chemiluminescent microparticle immunoassay of alpha-fetoprotein. Methods Serum alpha-fetoprotein was determined using the ARCHITECT alpha-fetoprotein assay. The estimation of alpha-fetoprotein recovery was carried out in samples prepared by diluting high-concentration alpha-fetoprotein serum with rheumatoid factor-positive or rheumatoid factor-negative serum. Paramagnetic microparticles coated with hepatitis B surface antigen-anti-HBs complexes were used to remove rheumatoid factor from the serum. Results The average recovery of alpha-fetoprotein was 88.4% and 93.8% in the rheumatoid factor-positive and rheumatoid factor-negative serum samples, respectively. The recovery of alpha-fetoprotein was significantly lower in the rheumatoid factor-positive serum samples than in the rheumatoid factor-negative serum samples. In two of five rheumatoid factor-positive samples, a large difference was found (9.8%) between the average alpha-fetoprotein recoveries in the serially diluted and initial recoveries. Fourteen rheumatoid factor-positive serum samples were pretreated with hepatitis B surface antigen-anti-HBs complex-coated paramagnetic microparticles. The alpha-fetoprotein concentrations measured in the pretreated samples increased significantly. Conclusions It was concluded that the alpha-fetoprotein chemiluminescent microparticle immunoassay is susceptible to interference by rheumatoid factor, leading to significantly lower results. Eliminating the incidence of negative interference from rheumatoid factor should be an important goal for immunoassay providers. In the meantime, laboratorians must remain alert to the negative interference by rheumatoid factor, and in some cases, pretreat rheumatoid factor-positive samples with blocking or absorbing reagents.

[Study of blending method for the extracts of herbal plants].

PubMed

Liu, Yongsuo; Cao, Min; Chen, Yuying; Hu, Yuzhu; Wang, Yiming; Luo, Guoan

2006-03-01

The irregularity in herbal plant composition is influenced by multiple factors. As for quality control of traditional Chinese medicine, the most critical challenge is to ensure the dosage content uniformity. This content uniformity can be improved by blending different batches of the extracts of herbal plants. Nonlinear least-squares regression was used to calculate the blending coefficient, which means no great absolute differences allowed for all ingredients. For traditional Chinese medicines, even relatively smaller differences could present to be very important for all the ingredients. The auto-scaling pretreatment was used prior to the calculation of the blending coefficients. The pretreatment buffered the characteristics of individual data for the ingredients in different batches, so an improved auto-scaling pretreatment method was proposed. With the improved auto-scaling pretreatment, the relative. differences decreased after blending different batches of extracts of herbal plants according to the reference samples. And the content uniformity control of the specific ingredients could be achieved by the error control coefficient. In the studies for the extracts of fructus gardeniae, the relative differences of all the ingredients is less than 3% after blending different batches of the extracts. The results showed that nonlinear least-squares regression can be used to calculate the blending coefficient of the herbal plant extracts.

Simplifying sample pretreatment: application of dried blood spot (DBS) method to blood samples, including postmortem, for UHPLC-MS/MS analysis of drugs of abuse.

PubMed

Odoardi, Sara; Anzillotti, Luca; Strano-Rossi, Sabina

2014-10-01

The complexity of biological matrices, such as blood, requires the development of suitably selective and reliable sample pretreatment procedures prior to their instrumental analysis. A method has been developed for the analysis of drugs of abuse and their metabolites from different chemical classes (opiates, methadone, fentanyl and analogues, cocaine, amphetamines and amphetamine-like substances, ketamine, LSD) in human blood using dried blood spot (DBS) and subsequent UHPLC-MS/MS analysis. DBS extraction required only 100μL of sample, added with the internal standards and then three droplets (30μL each) of this solution were spotted on the card, let dry for 1h, punched and extracted with methanol with 0.1% of formic acid. The supernatant was evaporated and the residue was then reconstituted in 100μL of water with 0.1% of formic acid and injected in the UHPLC-MS/MS system. The method was validated considering the following parameters: LOD and LOQ, linearity, precision, accuracy, matrix effect and dilution integrity. LODs were 0.05-1ng/mL and LOQs were 0.2-2ng/mL. The method showed satisfactory linearity for all substances, with determination coefficients always higher than 0.99. Intra and inter day precision, accuracy, matrix effect and dilution integrity were acceptable for all the studied substances. The addition of internal standards before DBS extraction and the deposition of a fixed volume of blood on the filter cards ensured the accurate quantification of the analytes. The validated method was then applied to authentic postmortem blood samples. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Microbial pretreatment of cotton stalks by Phanerochaete chrysosporium for bioethanol production

NASA Astrophysics Data System (ADS)

Shi, Jian

Lignocellulosic biomass has been recognized as a widespread, potentially low cost renewable source of mixed sugars for fermentation to fuel ethanol. Pretreatment, as the first step towards conversion of lignocellulose to ethanol, remains one of the main barriers to technical and commercial success of the processing technology. Existing pretreatment methods have largely been developed on the basis of physiochemical technologies which are considered relatively expensive and usually involve adverse environmental impacts. In this study, an environmentally benign alternative, microbial pretreatment using Phanerochaete chrysosporium, was explored to degrade lignin in cotton stalks and facilitate their conversion into ethanol. Two submerged liquid pretreatment techniques (SmC), shallow stationary and agitated cultivation, at three inorganic salt concentrations (no salts, modified salts without Mn2+, modified salts with Mn2+) were compared by evaluating their pretreatment efficiencies. Shallow stationary cultivation with no salt was superior to other pretreatment conditions and gave 20.7% lignin degradation along with 76.3% solids recovery and 29.0% carbohydrate availability over a 14 day period. The influence of substrate moisture content (65%, 75% and 80% M.C. wet-basis), inorganic salt concentration (no salts, modified salts without Mn2+ , modified salts with Mn2+) and culture time (0-14 days) on pretreatment effectiveness in solid state (SSC) systems was also examined. It was shown that solid state cultivation at 75% M.C. without salts was the most preferable pretreatment resulting in 27.6% lignin degradation, 71.1% solids recovery and 41.6% carbohydrate availability over a period of 14 days. A study on hydrolysis and fermentation of cotton stalks treated microbially using the most promising SmC (shallow stationary, no salts) and SSC (75% moisture content, no salts) methods resulted in no increase in cellulose conversion with direct enzyme application (10.98% and 3.04% for SmC and SSC pretreated samples, respectively) compared with untreated cotton stalk samples (17.93%). Washing of pretreated cotton stalks alone caused no significant increase in cellulose conversion. However, a heat treatment (autoclaving) followed by washing remarkably improved (P<0.05) cellulose conversion to 14.94% and 17.81% for SmC and SSC pretreatment, respectively. Mathematical models describing holocellulose consumption, lignin degradation, cellulase and ligninolytic enzyme production, and oxygen uptake associated with the growth of P. chrysosporium during 14 days fungal pretreatment were developed. For SmC pretreatment, model parameters were estimated by nonlinear regression and validated using an independent set of experimental data. Models yielded sufficiently accurate predictions for holocellulose consumption (R2=0.9772 and 0.9837, 1d and 3d oxygen flushing, respectively), lignin degradation (R2=0.9879 and 0.8682) and ligninolytic enzyme production (R2=0.8135 and 0.9693) under both 1 and 3d oxygen flushing conditions. However, the prediction capabilities for fungal growth (1d and 3d), cellulase production (3d) and oxygen uptake (3d) were limited. For SSC, the models were established in three phases (I: day 0-4, II: day 4-7, III: day 7-14). After validation it was shown that the developed models can yield sufficiently accurate predictions for fungal growth (R 2=0.9724), holocellulose consumption (R2=0.9686), lignin degradation (R2=0.9309) and ligninolytic enzyme production (R2=0.9203); however predictions of cellulase production were fair (R2=0.6133). Although significant delignification occurred during fungal pretreatment indicating the presence of ligninolytic enzymes, common spectrophotometric enzyme assays failed to detect lignin peroxidase (LiP) and manganese peroxidase (MnP) activities in fungal pretreatment cultures. Efforts were made to overcome the drawbacks of standardized assays by performing protein gel electrophoresis and crude enzyme delignification studies. Results from this research are expected to be beneficial in the development of pretreatment technologies that are environment friendly and utilize naturally occurring microorganisms.

Methods for pretreating biomass

DOEpatents

Balan, Venkatesh; Dale, Bruce E; Chundawat, Shishir; Sousa, Leonardo

2017-05-09

A method for pretreating biomass is provided, which includes, in a reactor, allowing gaseous ammonia to condense on the biomass and react with water present in the biomass to produce pretreated biomass, wherein reactivity of polysaccharides in the biomass is increased during subsequent biological conversion as compared to the reactivity of polysaccharides in biomass which has not been pretreated. A method for pretreating biomass with a liquid ammonia and recovering the liquid ammonia is also provided. Related systems which include a biochemical or biofuel production facility are also disclosed.

Biphasic microreactor for efficient membrane protein pretreatment with a combination of formic acid assisted solubilization, on-column pH adjustment, reduction, alkylation, and tryptic digestion.

PubMed

Zhao, Qun; Liang, Yu; Yuan, Huiming; Sui, Zhigang; Wu, Qi; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2013-09-17

Combining good dissolving ability of formic acid (FA) for membrane proteins and excellent complementary retention behavior of proteins on strong cation exchange (SCX) and strong anion exchange (SAX) materials, a biphasic microreactor was established to pretreat membrane proteins at microgram and even nanogram levels. With membrane proteins solubilized by FA, all of the proteomics sample processing procedures, including protein preconcentration, pH adjustment, reduction, and alkylation, as well as tryptic digestion, were integrated into an "SCX-SAX" biphasic capillary column. To evaluate the performance of the developed microreactor, a mixture of bovine serum albumin, myoglobin, and cytochrome c was pretreated. Compared with the results obtained by the traditional in-solution process, the peptide recovery (93% vs 83%) and analysis throughput (3.5 vs 14 h) were obviously improved. The microreactor was further applied for the pretreatment of 14 μg of membrane proteins extracted from rat cerebellums, and 416 integral membrane proteins (IMPs) (43% of total protein groups) and 103 transmembrane peptides were identified by two-dimensional nanoliquid chromatography-electrospray ionization tandem mass spectrometry (2D nano-LC-ESI-MS/MS) in triplicate analysis. With the starting sample preparation amount decreased to as low as 50 ng, 64 IMPs and 17 transmembrane peptides were identified confidently, while those obtained by the traditional in-solution method were 10 and 1, respectively. All these results demonstrated that such an "SCX-SAX" based biphasic microreactor could offer a promising tool for the pretreatment of trace membrane proteins with high efficiency and throughput.

Measurement of Outgassing Rates of Steels.

PubMed

Park, Chongdo; Kim, Se-Hyun; Ki, Sanghoon; Ha, Taekyun; Cho, Boklae

2016-12-13

Steels are commonly used materials in the fabrication of vacuum systems because of their good mechanical, corrosion, and vacuum properties. A variety of steels meet the criterion of low outgassing required for high or ultrahigh vacuum applications. However, a given material can present different outgassing rates depending on its manufacturing process or the various pretreatment processes involved during the fabrication. Thus, the measurement of outgassing rates is highly desirable for a specific vacuum application. For this reason, the rate-of-pressure rise (RoR) method is often used to measure the outgassing of hydrogen after bakeout. In this article, a detailed description of the design and execution of the experimental protocol involved in the RoR method is provided. The RoR method uses a spinning rotor gauge to minimize errors that stem from outgassing or the pumping action of a vacuum gauge. The outgassing rates of two ordinary steels (stainless steel and mild steel) were measured. The measurements were made before and after the heat pretreatment of the steels. The heat pretreatment of steels was performed to reduce the outgassing. Extremely low rates of outgassing (on the order of 10 - 11 Pa m 3 sec - 1 m - 2 ) can be routinely measured using relatively small samples.

Effects of pre-treatment technologies on quantity and quality of source-sorted municipal organic waste for biogas recovery.

PubMed

Hansen, Trine Lund; Jansen, Jes la Cour; Davidsson, Asa; Christensen, Thomas Højlund

2007-01-01

Source-sorted municipal organic waste collected from different dwelling types in five Danish cities and pre-treated at three different plants was sampled and characterized several times during one year to investigate the origin of any differences in composition of the pre-treated waste introduced by city, pre-treatment technology, dwelling type or annual season. The investigated pre-treatment technologies were screw press, disc screen and shredder+magnet. The average quantity of pre-treated organic waste (biomass) produced from the incoming waste varied between the investigated pre-treatment technologies: 59%, 66% and 98% wet weight, respectively (41%, 34% and 2% reject, respectively). The pre-treatment technologies showed differences with respect to distribution of the chemical components in the waste between the biomass and the rejected material (reject), especially for dry matter, ash, collection bag material (plastic or paper) and easily degradable organic matter. Furthermore, the particle size of the biomass was related to the pre-treatment technology. The content of plastic in the biomass depended both on the actual collection bag material used in the system and the pre-treatment technology. The sampled reject consisted mostly of organic matter. For cities using plastic bags for the source-separated organic waste, the expected content of plastic in the reject was up to 10% wet weight (in some cases up to 20%). Batch tests for methane potential of the biomass samples showed only minor variations caused by the factors city, pre-treatment technology, dwelling type and season when based on the VS content of the waste (overall average 459STPm(3)/tVS). The amount of methane generated from 1t of collected waste was therefore mainly determined by the efficiency of the chosen pre-treatment technology described by the mass distribution of the incoming waste between biomass and reject.

Ionic liquid pretreatment of poplar wood at room temperature: swelling and incorporation of nanoparticles.

PubMed

Lucas, Marcel; Macdonald, Brian A; Wagner, Gregory L; Joyce, Stephen A; Rector, Kirk D

2010-08-01

Lignocellulosic biomass offers economic and environmental advantages over corn starch for biofuels production. However, its fractionation currently requires energy-intensive pretreatments, due to the lignin chemical resistance and complex cell wall structure. Recently, ionic liquids have been used to dissolve biomass at high temperatures. In this study, thin sections of poplar wood were swollen by ionic liquid (1-ethyl-3-methylimidazolium acetate) pretreatment at room temperature. The samples contract when rinsed with deionized water. The controlled expansion and contraction of the wood structure can be used to incorporate enzymes and catalysts deep into the wood structure for improved pretreatments and accelerated cellulose hydrolysis. As a proof of concept, silver and gold nanoparticles of diameters ranging from 20 to 100 nm were incorporated at depths up to 4 mum. Confocal surface-enhanced Raman images at different depths show that a significant number of nanoparticles were incorporated into the pretreated sample, and they remained on the samples after rinsing. Quantitative X-ray fluorescence microanalyses indicate that the majority of nanoparticle incorporation occurs after an ionic liquid pretreatment of less than 1 h. In addition to improved pretreatments, the incorporation of materials and chemicals into wood and paper products enables isotope tracing, development of new sensing, and imaging capabilities.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Webb-Robertson, Bobbie-Jo; Kim, Young -Mo; Zink, Erika M.

Urease pre-treatment of urine has been utilized since the early 1960s to remove high levels of urea from samples prior to further processing and analysis by gas chromatography-mass spectrometry (GC-MS). Aside from the obvious depletion or elimination of urea, the effect, if any, of urease pre-treatment on the urinary metabolome has not been studied in detail. Here, we report the results of three separate but related experiments that were designed to assess possible indirect effects of urease pre-treatment on the urinary metabolome as measured by GC-MS. In total, 235 GC-MS analyses were performed and over 106 identified and 200 unidentifiedmore » metabolites were quantified across the three experiments. The results showed that data from urease pre-treated samples 1) had the same or lower coefficients of variance among reproducibly detected metabolites, 2) more accurately reflected quantitative differences and the expected ratios among different urine volumes, and 3) increased the number of metabolite identifications. Altogether, we observed no negative consequences of urease pre-treatment. In contrast, urease pretreatment enhanced the ability to distinguish between volume-based and biological sample types compared to no treatment. Taken together, these results show that urease pretreatment of urine offers multiple beneficial effects that outweigh any artifacts that may be introduced to the data in urinary metabolomics analyses.« less

Assessment of chemical and material contamination in waste wood fuels--A case study ranging over nine years.

PubMed

Edo, Mar; Björn, Erik; Persson, Per-Erik; Jansson, Stina

2016-03-01

The increased demand for waste wood (WW) as fuel in Swedish co-combustion facilities during the last years has increased the import of this material. Each country has different laws governing the use of chemicals and therefore the composition of the fuel will likely change when combining WW from different origins. To cope with this, enhanced knowledge is needed on WW composition and the performance of pre-treatment techniques for reduction of its contaminants. In this study, the chemical and physical characteristics of 500 WW samples collected at a co-combustion facility in Sweden between 2004 and 2013 were investigated to determine the variation of contaminant content over time. Multivariate data analysis was used for the interpretation of the data. The concentrations of all the studied contaminants varied widely between sampling occasions, demonstrating the highly variable composition of WW fuels. The efficiency of sieving as a pre-treatment measure to reduce the levels of contaminants was not sufficient, revealing that sieving should be used in combination with other pre-treatment methods. The results from this case study provide knowledge on waste wood composition that may benefit its management. This knowledge can be applied for selection of the most suitable pre-treatments to obtain high quality sustainable WW fuels. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

Comparative study of corn stover pretreated by dilute acid and cellulose solvent-based lignocellulose fractionation: Enzymatic hydrolysis, supramolecular structure, and substrate accessibility.

PubMed

Zhu, Zhiguang; Sathitsuksanoh, Noppadon; Vinzant, Todd; Schell, Daniel J; McMillan, James D; Zhang, Y-H Percival

2009-07-01

Liberation of fermentable sugars from recalcitrant biomass is among the most costly steps for emerging cellulosic ethanol production. Here we compared two pretreatment methods (dilute acid, DA, and cellulose solvent and organic solvent lignocellulose fractionation, COSLIF) for corn stover. At a high cellulase loading [15 filter paper units (FPUs) or 12.3 mg cellulase per gram of glucan], glucan digestibilities of the corn stover pretreated by DA and COSLIF were 84% at hour 72 and 97% at hour 24, respectively. At a low cellulase loading (5 FPUs per gram of glucan), digestibility remained as high as 93% at hour 24 for the COSLIF-pretreated corn stover but reached only approximately 60% for the DA-pretreated biomass. Quantitative determinations of total substrate accessibility to cellulase (TSAC), cellulose accessibility to cellulase (CAC), and non-cellulose accessibility to cellulase (NCAC) based on adsorption of a non-hydrolytic recombinant protein TGC were measured for the first time. The COSLIF-pretreated corn stover had a CAC of 11.57 m(2)/g, nearly twice that of the DA-pretreated biomass (5.89 m(2)/g). These results, along with scanning electron microscopy images showing dramatic structural differences between the DA- and COSLIF-pretreated samples, suggest that COSLIF treatment disrupts microfibrillar structures within biomass while DA treatment mainly removes hemicellulose. Under the tested conditions COSLIF treatment breaks down lignocellulose structure more extensively than DA treatment, producing a more enzymatically reactive material with a higher CAC accompanied by faster hydrolysis rates and higher enzymatic digestibility. (c) 2009 Wiley Periodicals, Inc.

Improvements of the Vis-NIRS Model in the Prediction of Soil Organic Matter Content Using Spectral Pretreatments, Sample Selection, and Wavelength Optimization

NASA Astrophysics Data System (ADS)

Lin, Z. D.; Wang, Y. B.; Wang, R. J.; Wang, L. S.; Lu, C. P.; Zhang, Z. Y.; Song, L. T.; Liu, Y.

2017-07-01

A total of 130 topsoil samples collected from Guoyang County, Anhui Province, China, were used to establish a Vis-NIR model for the prediction of organic matter content (OMC) in lime concretion black soils. Different spectral pretreatments were applied for minimizing the irrelevant and useless information of the spectra and increasing the spectra correlation with the measured values. Subsequently, the Kennard-Stone (KS) method and sample set partitioning based on joint x-y distances (SPXY) were used to select the training set. Successive projection algorithm (SPA) and genetic algorithm (GA) were then applied for wavelength optimization. Finally, the principal component regression (PCR) model was constructed, in which the optimal number of principal components was determined using the leave-one-out cross validation technique. The results show that the combination of the Savitzky-Golay (SG) filter for smoothing and multiplicative scatter correction (MSC) can eliminate the effect of noise and baseline drift; the SPXY method is preferable to KS in the sample selection; both the SPA and the GA can significantly reduce the number of wavelength variables and favorably increase the accuracy, especially GA, which greatly improved the prediction accuracy of soil OMC with Rcc, RMSEP, and RPD up to 0.9316, 0.2142, and 2.3195, respectively.

Spatially resolved in vivo plant metabolomics by laser ablation-based mass spectrometry imaging (MSI) techniques: LDI-MSI and LAESI

PubMed Central

Bartels, Benjamin; Svatoš, Aleš

2015-01-01

This short review aims to summarize the current developments and applications of mass spectrometry-based methods for in situ profiling and imaging of plants with minimal or no sample pre-treatment or manipulation. Infrared-laser ablation electrospray ionization and UV-laser desorption/ionization methods are reviewed. The underlying mechanisms of the ionization techniques–namely, laser ablation of biological samples and electrospray ionization–as well as variations of the LAESI ion source for specific targets of interest are described. PMID:26217345

Determination of bisphenol A in human serum by high-performance liquid chromatography with multi-electrode electrochemical detection.

PubMed

Inoue, K; Kato, K; Yoshimura, Y; Makino, T; Nakazawa, H

2000-11-10

A simple and sensitive method using high-performance liquid chromatography with multi-electrode electrochemical detection (HPLC-ED) including a coulometric array of four electrochemical sensors has been developed for the determination of bisphenol A in water and human serum. For good separation and detection of bisphenol A, a CAPCELL PAK UG 120 C18 reversed-phase column and a mobile phase consisting of 0.3% phosphoric acid-acetonitrile (60:40) were used. The detection limit obtained by the HPLC-ED method was 0.01 ng/ml (0.5 pg), which was more than 3000-times higher than the detection limit obtained by the ultraviolet (UV) method, and more than 200-times higher than the detection limit obtained by the fluorescence (FL) method. Bisphenol A in water and serum samples was pretreated by solid-phase extraction (SPE) after removing possible contamination derived from a plastic SPE cartridges and water used for the pretreatment. A trace amount (ND approximately 0.013 ng/ml) of bisphenol A was detected from the parts of cartridges (filtration column, sorbent bed and frits) by extraction with methanol, and it was completely removed by washing with at least 15 ml of methanol in the operation process. The concentrations of bisphenol A in tap water and Milli-Q-purified water were found to be 0.01 and 0.02 ng/ml, respectively. For that reason, bisphenol A-free water was made to trap bisphenol A in water using an Empore disk. In every pretreatment, SPE methods using bisphenol A-free water and washing with 15 ml of methanol were done in water and serum samples. The yields obtained from the recovery tests using water to which 0.5 or 0.05 ng/ml of bisphenol A was added were 83.8 to 98.2%, and the RSDs were 3.4 to 6.1%, respectively. The yields obtained from the recovery tests by OASIS HLB using serum to which 1.0 ng/ml or 0.1 ng/ml of bisphenol A was added were 79.0% and 87.3%, and the RSDs were 5.1% and 13.5%, respectively. The limits of quantification in water and serum sample were 0.01 ng/ml and 0.05 ng/ml, respectively. The method was applied to the determination of bisphenol A in healthy human serum sample, and the obtained detection was 0.32 ng/ml. From these results, the HPLC-ED method should be the most useful in the determination of bisphenol A at low concentration levels in water and biological samples.

Microbiological test results of the environmental control and life support systems vapors compression distillation subsystem recycle tank components following various pretreatment protocols

NASA Technical Reports Server (NTRS)

Huff, Tim

1993-01-01

Microbiological samples were collected from the recycle tank of the vapor compression distillation (VCD) subsystem of the water recovery test at NASA MSFC following a 68-day run. The recycle tank collects rejected urine brine that was pretreated with a commercially available oxidant (Oxone) and sulfuric acid and pumps it back to the processing component of the VCD. Samples collected included a water sample and two swab samples, one from the particulate filter surface and a second from material floating on the surface of the water. No bacteria were recovered from the water sample. Both swab samples contained a spore-forming bacterium, Bacillus insolitus. A filamentous fungus was isolated from the floating material. Approximately 1 month after the pretreatment chemicals were changed to sodium hypochlorite and sulfuric acid, a swab of the particulate filter was again analyzed for microbial content. One fungus was isolated, and spore-forming bacteria were observed. These results indicate the inability of these pretreatments to inhibit surface attachment. The implications of the presence of these organisms are discussed.

Maleic acid treatment of biologically detoxified corn stover liquor.

PubMed

Kim, Daehwan; Ximenes, Eduardo A; Nichols, Nancy N; Cao, Guangli; Frazer, Sarah E; Ladisch, Michael R

2016-09-01

Elimination of microbial and enzyme inhibitors from pretreated lignocellulose is critical for effective cellulose conversion and yeast fermentation of liquid hot water (LHW) pretreated corn stover. In this study, xylan oligomers were hydrolyzed using either maleic acid or hemicellulases, and other soluble inhibitors were eliminated by biological detoxification. Corn stover at 20% (w/v) solids was LHW pretreated LHW (severity factor: 4.3). The 20% solids (w/v) pretreated corn stover derived liquor was recovered and biologically detoxified using the fungus Coniochaeta ligniaria NRRL30616. After maleic acid treatment, and using 5 filter paper units of cellulase/g glucan (8.3mg protein/g glucan), 73% higher cellulose conversion from corn stover was obtained for biodetoxified samples compared to undetoxified samples. This corresponded to 87% cellulose to glucose conversion. Ethanol production by yeast of pretreated corn stover solids hydrolysate was 1.4 times higher than undetoxified samples, with a reduction of 3h in the fermentation lag phase. Copyright © 2016 Elsevier Ltd. All rights reserved.

Improved volatile fatty acid and biomethane production from lipid removed microalgal residue (LRμAR) through pretreatment.

PubMed

Suresh, Arumuganainar; Seo, Charles; Chang, Ho Nam; Kim, Yeu-Chun

2013-12-01

Renewable energy from lipid removed microalgal residues (LRμARs) serves as a promising tool for sustainable development of the microalgal biodiesel industry. Hence, in this study, LRμAR from Ettlia sp. was characterized for its physico-biochemical parameters, and applied to various pretreatment to increase the biodegradability and used in batch experiments for the production of volatile fatty acids (VFA) and biomethane. After various pretreatments, the soluble organic matters were increased at a maximum of 82% in total organic matters in alkali-autoclaved sample. In addition, VFA and methane production was enhanced by 30% and 40% in alkali-sonicated and alkali-autoclaved samples, respectively. Methane heating value was recovered at maximum of 6.6 MJ kg(-1)VS in alkali-autoclaved conditions with comparison to non-pretreated samples. The pretreatment remarkably improved LRμAR solubilization and enhanced VFA and biomethane production, which holds immense potential to eventually reduce the cost of algal biodiesel. Copyright © 2013 Elsevier Ltd. All rights reserved.

Facile synthesis of poly(ionic liquid)-bonded magnetic nanospheres as a high-performance sorbent for the pretreatment and determination of phenolic compounds in water samples.

PubMed

Bi, Wentao; Wang, Man; Yang, Xiaodi; Row, Kyung Ho

2014-07-01

Poly(ionic liquid)-bonded magnetic nanospheres were easily synthesized and applied to the pretreatment and determination of phenolic compounds in water samples, which have detrimental effects on water quality and the health of living beings. The high affinity of poly(ionic liquid)s toward the target compounds as well as the magnetic behavior of Fe3 O4 were combined in this material to provide an efficient and simple magnetic solid-phase extraction approach. The adsorption behavior of the poly(ionic liquid)-bonded magnetic nanospheres was examined to optimize the synthesis. Different parameters affecting the magnetic solid-phase extraction of phenolic compounds were assessed in terms of adsorption and recovery. Under the optimal conditions, the proposed method showed excellent detection sensitivity with limits of detection in the range of 0.3-0.8 ng/mL and precision in the range of 1.2-3.3%. This method was also applied successfully to the analysis of real water samples; good spiked recoveries over the range of 82.5-99.2% were obtained. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Exploring accessibility of pretreated poplar cell walls by measuring dynamics of fluorescent probes.

PubMed

Paës, Gabriel; Habrant, Anouck; Ossemond, Jordane; Chabbert, Brigitte

2017-01-01

The lignocellulosic cell wall network is resistant to enzymatic degradation due to the complex chemical and structural features. Pretreatments are thus commonly used to overcome natural recalcitrance of lignocellulose. Characterization of their impact on architecture requires combinatory approaches. However, the accessibility of the lignocellulosic cell walls still needs further insights to provide relevant information. Poplar specimens were pretreated using different conditions. Chemical, spectral, microscopic and immunolabeling analysis revealed that poplar cell walls were more altered by sodium chlorite-acetic acid and hydrothermal pretreatments but weakly modified by soaking in aqueous ammonium. In order to evaluate the accessibility of the pretreated poplar samples, two fluorescent probes (rhodamine B-isothiocyanate-dextrans of 20 and 70 kDa) were selected, and their mobility was measured by using the fluorescence recovery after photobleaching (FRAP) technique in a full factorial experiment. The mobility of the probes was dependent on the pretreatment type, the cell wall localization (secondary cell wall and cell corner middle lamella) and the probe size. Overall, combinatory analysis of pretreated poplar samples showed that even the partial removal of hemicellulose contributed to facilitate the accessibility to the fluorescent probes. On the contrary, nearly complete removal of lignin was detrimental to accessibility due to the possible cellulose-hemicellulose collapse. Evaluation of plant cell wall accessibility through FRAP measurement brings further insights into the impact of physicochemical pretreatments on lignocellulosic samples in combination with chemical and histochemical analysis. This technique thus represents a relevant approach to better understand the effect of pretreatments on lignocellulose architecture, while considering different limitations as non-specific interactions and enzyme efficiency.

Air radon equilibrium factor measurement in a Waste Water Pre-Treatment Plant

NASA Astrophysics Data System (ADS)

Martinez, J. E.; Juste, B.; Ortiz, J.; Martorell, S.; Verdu, G.

2017-11-01

We analyze in this paper a Waste Water Pre-Treatment Plant (WWTP) located at the Mediterranean coast with air radon concentration above Spanish action level (600 Bq per cubic meter). This paper presents a method for radon equilibrium determination by gamma spectrometry measuring of the radon progeny concentrations in the air, in order to estimate WWTP workers effective dose more exactly. The method is based on simultaneous sampling of air through a filter paper and alpha spectrometry measurement of radon activity concentration in the air. According to the measured radon activity concentration in the air of 368±45 Bq/m3 the equilibrium factor between radon and progenies is estimated to be F=0.27, which is in good agreement with expected values.

Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

PubMed

Xu, Hui; Liao, Ying; Yao, Jinrong

2007-10-05

A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

Methods of pretreating comminuted cellulosic material with carbonate-containing solutions

DOEpatents

Francis, Raymond

2012-11-06

Methods of pretreating comminuted cellulosic material with an acidic solution and then a carbonate-containing solution to produce a pretreated cellulosic material are provided. The pretreated material may then be further treated in a pulping process, for example, a soda-anthraquinone pulping process, to produce a cellulose pulp. The pretreatment solutions may be extracted from the pretreated cellulose material and selectively re-used, for example, with acid or alkali addition, for the pretreatment solutions. The resulting cellulose pulp is characterized by having reduced lignin content and increased yield compared to prior art treatment processes.

Concurrent Lactic and Volatile Fatty Acid Analysis of Microbial Fermentation Samples by Gas Chromatography with Heat Pre-treatment.

PubMed

Darwin; WipaCharles; Cord-Ruwisch, Ralf

2018-01-01

Organic acid analysis of fermentation samples can be readily achieved by gas chromatography (GC), which detects volatile organic acids. However, lactic acid, a key fermentation acid is non-volatile and can hence not be quantified by regular GC analysis. However the addition of periodic acid to organic acid samples has been shown to enable lactic acid analysis by GC, as periodic acid oxidizes lactic acid to the volatile acetaldehyde. Direct GC injection of lactic acid standards and periodic acid generated inconsistent and irreproducible peaks, possibly due to incomplete lactic acid oxidation to acetaldehyde. The described method is developed to improve lactic acid analysis by GC by using a heat treated derivatization pre-treatment, such that it becomes independent of the retention time and temperature selection of the GC injector. Samples containing lactic acid were amended by periodic acid and heated in a sealed test tube at 100°C for at least 45 min before injecting it to the GC. Reproducible and consistent peaks of acetaldehyde were obtained. Simultaneous determination of lactic acid, acetone, ethanol, butanol, volatile fatty acids could also be accomplished by applying this GC method, enabling precise and convenient organic acid analysis of biological samples such as anaerobic digestion and fermentation processes. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

[Determination of multi-element contents in gypsum by ICP-AES].

PubMed

Guo, Zhong-bao; Bai, Yong-zhi; Cui, Jin-hua; Mei, Yi-fei; Ma, Zhen-zhu

2014-08-01

The content of multi-element in gypsum was determined by ICP-AES. The sample was pretreated by acid-soluble method or alkali-fusion method. Acid-soluble method is suitable for the determination of CaO, SOs, Al2O3, Fe2O3, MgO, K2O, Na2O, TiO2, P2O5, MnO, SrO and BaO. Alkali-fusion method is suitable for the determination of CaO, SO3, SiO2, Al2O3, Fe2O3, MgO, TiO2, P2O5, MnO, SrO, BaO and B2O3. Different series standard solutions were prepared considering the properties and content of elements and solution matrix. The limit of detection and quantification were confirmed for each element under their best analysis spectral lines. The recoveries of the two pretreatment methods were from 93% to 110%, besides that for TiO2 was 81%-87% as pretreated by acid-soluble method. All RSDs (n=6) of tests were from 0.70%-3.42%. The accuracies of CaO and SO3 with ICP-AES method were less than the chemical analysis method. The determination of CaO and SO3 with ICP-AES method is only suitable for the case of low accuracy requirement. The results showed that the method can be used for the determination of multi-element contents in gypsum, with simple operation, fast analysis and reliable results. Total elements can be analysed with both acid-soluble method and alkali-fusion method.

Comparison study of two procedures for the determination of emamectin benzoate in medicated fish feed.

PubMed

Farer, Leslie J; Hayes, John M

2005-01-01

A new method has been developed for the determination of emamectin benzoate in fish feed. The method uses a wet extraction, cleanup by solid-phase extraction, and quantitation and separation by liquid chromatography (LC). In this paper, we compare the performance of this method with that of a previously reported LC assay for the determination of emamectin benzoate in fish feed. Although similar to the previous method, the new procedure uses a different sample pretreatment, wet extraction, and quantitation method. The performance of the new method was compared with that of the previously reported method by analyses of 22 medicated feed samples from various commercial sources. A comparison of the results presented here reveals slightly lower assay values obtained with the new method. Although a paired sample t-test indicates the difference in results is significant, this difference is within the method precision of either procedure.

UPT scenarios: Implications for system reliability

NASA Technical Reports Server (NTRS)

Walsh, Daniel W.

1992-01-01

The objective of this project was to examine the corrosion resistance of 316L stainless steel in several urine pre-treat solutions. Four solutions were examined: untreated urine (control); urine pretreated with oxone (potassium peroxymonosulfate sulfate); urine pretreated with sodium hypochlorite (NaOCl); and urine pretreated with ozone (O3). In accordance with current procedures, all solutions but the control were acidified to a pH of 2.5 using sulfuric acid--this suppresses the generation of ammonia in the solutions and is intended to limit microbial growth. Welded and unwelded coupons were exposed to each solution. In addition, Titanium coupons (welded and unwelded) were exposed to biologically active environmental control and life support system (ECLSS) water. Microbial attachment and biofilm growth were monitored. Ozone was examined as a biocide/oxidizer/corrosion preventative (simultaneous addition) and as a remediation method (added one week after exposure). In an unrelated effort, HP 9-4-30 coupons were exposed to biologically active solutions. Corrosion rates for welded and unwelded samples were determined--results were correlated to the ongoing HP 9-4-30 weldment stress corrosion study.

The Impact of Post-Pretreatment Conditioning on Enzyme Accessibility and Water Interactions in Alkali Pretreated Rice Straw

NASA Astrophysics Data System (ADS)

Karuna, Nardrapee

Rice straw, a high-abundance lignocellulosic residue from rice production has tremendous potential as a feedstock for biofuel production in California. In this study, the impact of post-alkali pretreatment conditioning schemes on enzyme saccharification efficiency was examined, particularly focusing on understanding resulting biomass compositional impacts on water interactions with the biomass and enzyme accessibility to the cellulose fraction. Rice straw was pretreated with sodium hydroxide and subsequently washed by two different conditions: 1) by extensive washing with distilled water to reduce the pH to the optimum for cellulases which is pH 5--6, and 2) immediate pH adjustment to pH 5--6 with hydrochloric acid before extensive washing with distilled water. The two post-pretreatment conditions gave significant differences in ash, acid-insoluble lignin, glucan and xylan compositions. Alkali pretreatment improved cellulase digestibility of rice straw, and water washing improved enzymatic digestibility more than neutralization. Hydrolysis reactions with a purified Trichoderma reesei Cel7A, a reducing-end specific cellulase, demonstrated that the differences in saccharification are likely due to differences in the accessibility of the cellulose fraction to the cellulolytic enzymes. Further analyses were conducted to study the mobility of the water associated with the rice straw samples by measuring T2 relaxation times of the water protons by 1H-Nuclear Magnetic Resonance (NMR) relaxometry. Results showed significant changes in water association with the rice straw due to the pretreatment and due to the two different post-pretreatment conditions. Pretreatment increased the amount of water at the surface of the rice straw samples as indicated by increased amplitude of the shortest T2 time peaks in the relaxation spectra. Moreover, the amount of water in the first T2 pool in the water washed sample was significantly greater than in the neutralized sample. These results suggest that the specific surface area of rice straw accessible to water protons was increased by the alkali pretreatment, likely due to solubilization of alkali-soluble components of the cell walls. Post-pretreatment processes resulted in differences in the specific surface area likely due to re-precipitation of alkali solubilized components during neutralization. The T2 relaxation times of the surface water pool in washed and raw rice straw were not significantly different, at 4.4 and 4.5 ms, respectively, but both T2 times were significantly shorter than that of the neutralized and then washed sample, at 5.5 ms. The expectation was that the T2 times of the surface water peaks would reflect differences in surface composition of the rice straw samples. Further analysis of surface composition is necessary to further interpret the shortest T2 times observed in the samples. The T2 spectra of the rice straw samples contained longer T2 time peaks that were interpreted as differences in porosity of the rice straw due to the treatments. Pretreatment caused physical changes to rice straw that impacted water organization (3 peaks to 4 peaks), but the amount of water in the peaks were greater in the washed rice straw than the neutralized rice straw suggesting that water-washed rice straw had more of the larger pores than the neutralized and then washed rice straw. One possible explanation is that the neutralization caused precipitation of alkali solubilized components that filled the volumes of the pores.

Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry.

PubMed

Urakami, K; Saito, Y; Fujiwara, Y; Watanabe, C; Umemoto, K; Godo, M; Hashimoto, K

2000-12-01

Thermal desorption (TD) techniques followed by capillary GC/MS were applied for the analysis of residual solvents in bulk pharmaceuticals. Solvents desorbed from samples by heating were cryofocused at the head of a capillary column prior to GC/MS analysis. This method requires a very small amount of sample and no sample pretreatment. Desorption temperature was set at the point about 20 degrees C higher than the melting point of each sample individually. The relative standard deviations of this method tested by performing six consecutive analyses of 8 different samples were 1.1 to 3.1%, and analytical results of residual solvents were in agreement with those obtained by direct injection of N,N-dimethylformamide solution of the samples into the GC. This novel TD/GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents in bulk pharmaceuticals.

Comparative techno-economic analysis of steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological pretreatments of corn stover.

PubMed

Baral, Nawa Raj; Shah, Ajay

2017-05-01

Pretreatment is required to destroy recalcitrant structure of lignocelluloses and then transform into fermentable sugars. This study assessed techno-economics of steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological pretreatments, and identified bottlenecks and operational targets for process improvement. Techno-economic models of these pretreatment processes for a cellulosic biorefinery of 113.5 million liters butanol per year excluding fermentation and wastewater treatment sections were developed using a modelling software-SuperPro Designer. Experimental data of the selected pretreatment processes based on corn stover were gathered from recent publications, and used for this analysis. Estimated sugar production costs ($/kg) via steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological methods were 0.43, 0.42, 0.65 and 1.41, respectively. The results suggest steam explosion and sulfuric acid pretreatment methods might be good alternatives at present state of technology and other pretreatment methods require research and development efforts to be competitive with these pretreatment methods. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

PubMed

Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

2016-03-04

Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Gas pressure assisted microliquid-liquid extraction coupled online to direct infusion mass spectrometry: a new automated screening platform for bioanalysis.

PubMed

Raterink, Robert-Jan; Witkam, Yoeri; Vreeken, Rob J; Ramautar, Rawi; Hankemeier, Thomas

2014-10-21

In the field of bioanalysis, there is an increasing demand for miniaturized, automated, robust sample pretreatment procedures that can be easily connected to direct-infusion mass spectrometry (DI-MS) in order to allow the high-throughput screening of drugs and/or their metabolites in complex body fluids like plasma. Liquid-Liquid extraction (LLE) is a common sample pretreatment technique often used for complex aqueous samples in bioanalysis. Despite significant developments that have been made in automated and miniaturized LLE procedures, fully automated LLE techniques allowing high-throughput bioanalytical studies on small-volume samples using direct infusion mass spectrometry, have not been matured yet. Here, we introduce a new fully automated micro-LLE technique based on gas-pressure assisted mixing followed by passive phase separation, coupled online to nanoelectrospray-DI-MS. Our method was characterized by varying the gas flow and its duration through the solvent mixture. For evaluation of the analytical performance, four drugs were spiked to human plasma, resulting in highly acceptable precision (RSD down to 9%) and linearity (R(2) ranging from 0.990 to 0.998). We demonstrate that our new method does not only allow the reliable extraction of analytes from small sample volumes of a few microliters in an automated and high-throughput manner, but also performs comparable or better than conventional offline LLE, in which the handling of small volumes remains challenging. Finally, we demonstrate the applicability of our method for drug screening on dried blood spots showing excellent linearity (R(2) of 0.998) and precision (RSD of 9%). In conclusion, we present the proof of principe of a new high-throughput screening platform for bioanalysis based on a new automated microLLE method, coupled online to a commercially available nano-ESI-DI-MS.

Simple and rapid quantification of vancomycin in serum, urine and peritoneal/pleural effusion via UHPLC-MS/MS applicable to personalized antibiotic dosing research.

PubMed

Javorska, Lenka; Krcmova, Lenka Kujovska; Solich, Petr; Kaska, Milan

2017-08-05

Management of the therapy of life-threatening bacterial infection is extremely based on an optimal antibiotic treatment. Achieving the correct vancomycin dosage in blood and target tissues can be complicated in special situations, e.g., where large fluid sequestration and/or acute renal failure occur. A UHPLC-MS/MS method operating in electrospray (ESI) positive ion mode was applied for the determination of vancomycin in serum, urine and peritoneal/pleural effusion. Sample pretreatment was composed of dilution and simple protein precipitation where only a small volume (50μL) of serum, urine or peritoneal/pleural effusion was required. The separation of vancomycin was performed on a Meteoric Core C18 BIO column (100×4.6mm, 2.7μm) by gradient elution with 0.1% formic acid in water and acetonitrile. The total time of analysis was 4.5min. The method was found to be linear in the range of 2-60μM (or 0.5-10μM) for serum, 0.27-10μM (or 2-60μM) for peritoneal/pleural effusion and 25-300μM for urine, which was adequate for the determination of vancomycin in patient samples. The intra- and inter-day precision was below 8% RSD, and accuracy was from 89 to 104%. The UHPLC/MS-MS method offers a fast and reliable approach to determine vancomycin concentrations in three different human body fluid samples (serum, urine and peritoneal/pleural effusion) with a simple sample pretreatment that was the same for all selected specimens. This method should be applicable to large sample series in clinical (pharmacokinetic/pharmacodynamic) studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Diethylstilbestrol in fish tissue determined through subcritical fluid extraction and with GC-MS

NASA Astrophysics Data System (ADS)

Qiao, Qinghui; Shi, Nianrong; Feng, Xiaomei; Lu, Jie; Han, Yuqian; Xue, Changhu

2016-06-01

As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol (DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane (R134a) extraction in combination with gas chromatography-mass spectrometry (GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C18 and NH2 solid phase extraction (SPE). Finally, the analyte was derived by heptafluorobutyric anhydride (HFBA), followed by GC-MS analysis. Response surface methodology (RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26°C; amount of co-solvent volume, 4.7 mL. Under this condition, at a spiked level of 1, 5, 10 μg kg-1, the mean recovery of DES was more than 90% with relative standard deviations (RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

Comparison of different pretreatment strategies for enzymatic hydrolysis of wheat and barley straw.

PubMed

Rosgaard, Lisa; Pedersen, Sven; Meyer, Anne S

2007-12-01

In biomass-to-ethanol processes a physico-chemical pretreatment of the lignocellulosic biomass is a critical requirement for enhancing the accessibility of the cellulose substrate to enzymatic attack. This report evaluates the efficacy on barley and wheat straw of three different pretreatment procedures: acid or water impregnation followed by steam explosion versus hot water extraction. The pretreatments were compared after enzyme treatment using a cellulase enzyme system, Celluclast 1.5 L from Trichoderma reesei, and a beta-glucosidase, Novozyme 188 from Aspergillus niger. Barley straw generally produced higher glucose concentrations after enzymatic hydrolysis than wheat straw. Acid or water impregnation followed by steam explosion of barley straw was the best pretreatment in terms of resulting glucose concentration in the liquid hydrolysate after enzymatic hydrolysis. When the glucose concentrations obtained after enzymatic hydrolyses were related to the potential glucose present in the pretreated residues, the highest yield, approximately 48% (g g-1), was obtained with hot water extraction pretreatment of barley straw; this pretreatment also produced highest yields for wheat straw, producing a glucose yield of approximately 39% (g g-1). Addition of extra enzyme (Celluclast 1.5 L+Novozyme 188) during enzymatic hydrolysis resulted in the highest total glucose concentrations from barley straw, 32-39 g L-1, but the relative increases in glucose yields were higher on wheat straw than on barley straw. Maldi-TOF MS analyses of supernatants of pretreated barley and wheat straw samples subjected to acid and water impregnation, respectively, and steam explosion, revealed that the water impregnated + steam-exploded samples gave a wider range of pentose oligomers than the corresponding acid-impregnated samples.

Progress in ethanol production from corn kernel by applying cooking pre-treatment.

PubMed

Voca, Neven; Varga, Boris; Kricka, Tajana; Curic, Duska; Jurisic, Vanja; Matin, Ana

2009-05-01

In order to improve technological properties of corn kernel for ethanol production, samples were treated with a hydrothermal pre-treatment of cooking (steaming), prior to drying. Two types of cooking process parameters were applied; steam pressure of 0.5 bars during a 10 min period, and steam pressure of 1.5 bars during a 30 min period. Afterwards, samples were dried at four different temperatures, 70, 90, 110 and 130 degrees C. Control sample was also submitted to the aforementioned drying parameters. Since the results showed that starch utilization, due to the gelatinization process, was considerably higher in the samples pre-treated before the ethanol production process, it was found that the cooking treatment had a positive effect on ethanol yield from corn kernel. Therefore, the highest ethanol yield was found in the corn kernel samples cooked for 30 min at steam pressure 1.5 bars and dried at 130 degrees C. Due to the similarity of processes used for starch fermentation, introduction of cooking pre-treatment will not significantly increase the overall ethanol production costs, whereas it will result in significantly higher ethanol yield.

Sensitive analysis of blonanserin, a novel antipsychotic agent, in human plasma by ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Ogawa, Tadashi; Hattori, Hideki; Kaneko, Rina; Ito, Kenjiro; Iwai, Masayo; Mizutani, Yoko; Arinobu, Tetsuya; Ishii, Akira; Suzuki, Osamu; Seno, Hiroshi

2010-01-01

A rapid and sensitive method for analysis of blonanserin in human plasma by ultra-performance liquid chromatography-tandem mass spectrometry is presented. After pretreatment of a plasma sample by solid-phase extraction, blonanserin was analyzed by the system with a C(18) column. This method gave satisfactory recovery rates, reproducibility, and good linearity of calibration curve in the range of 0.01-10.0 ng/mL for quality control samples spiked with blonanserin. The detection limit was as low as 1 pg/mL. This method seems very useful in forensic and clinical toxicology and pharmacokinetic studies.

Pretreatment methods for bioethanol production.

PubMed

Xu, Zhaoyang; Huang, Fang

2014-09-01

Lignocellulosic biomass, such as wood, grass, agricultural, and forest residues, are potential resources for the production of bioethanol. The current biochemical process of converting biomass to bioethanol typically consists of three main steps: pretreatment, enzymatic hydrolysis, and fermentation. For this process, pretreatment is probably the most crucial step since it has a large impact on the efficiency of the overall bioconversion. The aim of pretreatment is to disrupt recalcitrant structures of cellulosic biomass to make cellulose more accessible to the enzymes that convert carbohydrate polymers into fermentable sugars. This paper reviews several leading acidic, neutral, and alkaline pretreatments technologies. Different pretreatment methods, including dilute acid pretreatment (DAP), steam explosion pretreatment (SEP), organosolv, liquid hot water (LHW), ammonia fiber expansion (AFEX), soaking in aqueous ammonia (SAA), sodium hydroxide/lime pretreatments, and ozonolysis are intensively introduced and discussed. In this minireview, the key points are focused on the structural changes primarily in cellulose, hemicellulose, and lignin during the above leading pretreatment technologies.

Quality of life and communication in orthognathic treatment.

PubMed

Catt, Susan L; Ahmad, Sofia; Collyer, Jeremy; Hardwick, Lauren; Shah, Nahush; Winchester, Lindsay

2018-06-01

The primary aim was to determine what, if any, relationships exist between communication and quality of life in patients receiving orthognathic treatment since this has not been explored. A secondary aim was to compare the Quality of Life (QoL) of a pre-treatment sample with those at 2 years post-surgery. A cross-sectional questionnaire method was used. Outpatient clinics providing orthognathic treatment at four UK hospital sites. Two separate samples of pre-treatment (n = 73) and 2-year post-surgery (n = 78) patients participated in the study. At clinic appointments, all eligible patients were invited to complete the Orthognathic Quality of Life Questionnaire (OQLQ), a previously validated condition-specific quality of life measure. At the same time, participants at the 2-year post-surgery stage also completed a second short questionnaire, the Communication Assessment Tool-Team (CAT-T), where they rated the quality of communication they had received during treatment. One hundred and fifty-one complete responses were received. The average age was 24.5 years (S.D. 9.77) and the majority (67%) were female in both groups. Statistically significant associations were found between QoL and quality of communication in the treated sample. Findings also showed a comparatively poorer QoL for the pre-treatment participants. This reduced QoL was more pronounced in females than males for all aspects except dentofacial appearance. There was an improvement in QoL for patients at 2 years post-surgery compared to pre-treatment. There is an association between QoL and quality of communication as reported by participants at 2 years post-surgery. These novel findings are similar to outcomes in other patient settings such as oncology, but further investigation is required to establish the direction of cause and effect.

Evaluating Predictors of Program Attrition among Women Mandated into Batterer Intervention Treatment

ERIC Educational Resources Information Center

Buttell, Frederick P.; Powers, Dolores; Wong, Asia

2012-01-01

Objective: The purpose of the present study was to evaluate pretreatment differences between treatment completers and dropouts among a large sample of women ordered into a 26-week batterer intervention program (BIP). Method: The study employed a nonequivalent, control-group design (comparing program completers to dropouts) in a secondary analysis…

Determination of molecular weight distributions in native and pretreated wood.

PubMed

Leskinen, Timo; Kelley, Stephen S; Argyropoulos, Dimitris S

2015-03-30

The analysis of native wood components by size-exclusion chromatography (SEC) is challenging. Isolation, derivatization and solubilization of wood polymers is required prior to the analysis. The present approach allowed the determination of molecular weight distributions of the carbohydrates and of lignin in native and processed woods, without preparative component isolation steps. For the first time a component selective SEC analysis of sawdust preparations was made possible by the combination of two selective derivatization methods, namely; ionic liquid assisted benzoylation of the carbohydrate fraction and acetobromination of the lignin in acetic acid media. These were optimized for wood samples. The developed method was thus used to examine changes in softwood samples after degradative mechanical and/or chemical treatments, such as ball milling, steam explosion, green liquor pulping, and chemical oxidation with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The methodology can also be applied to examine changes in molecular weight and lignin-carbohydrate linkages that occur during wood-based biorefinery operations, such as pretreatments, and enzymatic saccharification. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biomass pretreatment

DOEpatents

Hennessey, Susan Marie; Friend, Julie; Elander, Richard T; Tucker, III, Melvin P

2013-05-21

A method is provided for producing an improved pretreated biomass product for use in saccharification followed by fermentation to produce a target chemical that includes removal of saccharification and or fermentation inhibitors from the pretreated biomass product. Specifically, the pretreated biomass product derived from using the present method has fewer inhibitors of saccharification and/or fermentation without a loss in sugar content.

Enhanced enzymatic saccharification of pretreated biomass using glycerol thermal processing (GTP).

PubMed

Zhang, Wei; Sathitsuksanoh, Noppadon; Barone, Justin R; Renneckar, Scott

2016-01-01

Biomass was heated (200-240°C) in the presence of glycerol, for 4-12 min, under shear to disrupt the native cell wall architecture. The impact of this method, named glycerol thermal processing (GTP), on saccharification efficiency of the hardwood Liquidambar styraciflua, and a control cellulose sample was studied as a function of treatment severity. Furthermore, the enzymatic conversion of samples with varying compositions was studied after extraction of the structural polymers. Interestingly, the sweet gum processed materials crystallinity index increased by 10% of the initial value. The experiments revealed that the residual lignin was not a barrier to limiting the digestibility of cellulose after pretreatment yielding up to 70% glucose based on the starting wood material. Further xylan removal greatly improved the cellulose hydrolysis rate, converting nearly 70% of the cellulose into glucose within 24h, and reaching 78% of ultimate glucan digestibility after 72 h. Copyright © 2015 Elsevier Ltd. All rights reserved.

Sampling method, storage and pretreatment of sediment affect AVS concentrations with consequences for bioassay responses.

PubMed

De Lange, H J; Van Griethuysen, C; Koelmans, A A

2008-01-01

Sediment treatment and sediment storage may alter sediment toxicity, and consequently biotic response. Purpose of our study was to combine these three aspects (treatment-toxicity-biotic response) in one integrated approach. We used Acid Volatile Sulfide (AVS) concentrations as a proxy of the disturbance of the sediment. AVS and Simultaneously Extracted Metal (SEM) concentrations were compared to bioassay responses with the freshwater benthic macroinvertebrate Asellus aquaticus. Storage conditions and sediment treatment affected AVS but not SEM levels. AVS can be used as a proxy for sediment disturbance. The best way to pretreat the sediment for use in a bioassay in order to maintain initial AVS conditions was to sample the sediment with an Ekman grab, immediately store it in a jar without headspace, and freeze it as soon as possible. In a survey using seven different sediments, bioassay responses of A. aquaticus were correlated with SEM and AVS characteristics.

Thermogravimetric study and kinetic analysis of fungal pretreated corn stover using the distributed activation energy model.

PubMed

Ma, Fuying; Zeng, Yelin; Wang, Jinjin; Yang, Yang; Yang, Xuewei; Zhang, Xiaoyu

2013-01-01

Non-isothermal thermogravimetry/derivative thermogravimetry (TG/DTG) measurements are used to determine pyrolytic characteristics and kinetics of lignocellulose. TG/DTG experiments at different heating rates with corn stover pretreated with monocultures of Irpex lacteus CD2 and Auricularia polytricha AP and their cocultures were conducted. Heating rates had little effect on the pyrolysis process, but the peak of weight loss rate in the DTG curves shifted towards higher temperature with heating rate. The maximum weight loss of biopretreated samples was 1.25-fold higher than that of the control at the three heating rates, and the maximum weight loss rate of the co-culture pretreated samples was intermediate between that of the two mono-cultures. The activation energies of the co-culture pretreated samples were 16-72 kJ mol(-1) lower than that of the mono-culture at the conversion rate range from 10% to 60%. This suggests that co-culture pretreatment can decrease activation energy and accelerate pyrolysis reaction thus reducing energy consumption. Copyright © 2012 Elsevier Ltd. All rights reserved.

High performance liquid chromatographic method for the determination of cetirizine and ambroxol in human plasma and urine--a boxcar approach.

PubMed

Dharuman, J; Vasudhevan, M; Ajithlal, T

2011-09-01

A column switching high performance liquid chromatographic method with estimable sensitivity and accuracy was developed for the determination of cetirizine and ambroxol in human plasma using nebivolol as the internal standard. Plasma samples were prepared by liquid-liquid extraction in methylene chloride and a mixture of diethylether (80:20, v/v). The extracted samples were injected into a multifunctional clean-up column Supelcosil LCABZ (50 mm × 4.6 mm, 5 μm particle size) using mobile phase 1 comprising acetonitrile-phosphate buffer (pH 3.5; 20 mM) (20:80, v/v). The eluate of cetirizine and ambroxol were separated to an analytical Kromasil C(8) micro bore column (50 mm × 0.3 mm, 5 μm particle size) via a column switching device. A Kromasil C(18) analytical column (250 mm × 2.1 mm, 5 μm particle size) was used as a separation column. Mobile phase 2 consisting acetonitrile-triethylamine (0.5%) in phosphate buffer (pH 3.5; 20mM) (55:45, v/v) was used for the compound elution. The eluents were detected at 230 nm with photodiode array detector. An aliquot of 150 μl of plasma sample was introduced into the pretreatment column via the auto sampler using mobile phase 1 at a flow rate of 0.5 ml/min, column switching valve being positioned at A. The pretreatment column retained cetirizine, ambroxol and nebivolol (IS) in the column leaving the residual proteins of plasma eluted in void volume and drained out. The switching valve was shifted to position B at 7.5 min. Cetirizine, ambroxol and IS were eluted from the pretreatment column between 7. 5 and 11.5 min and introduced to the concentration column. Finally, cetirizine, ambroxol and IS were introduced to the separation column by switching valve using mobile phase 2 at a flow rate of 0.4 ml/min. During the analysis the pretreatment column was washed for the next analysis and resume to the position A. The total run time was 25 min for a sample. The procedure was repeated for urine analysis also. The method was linear from 2 to 450 ng/ml and 7-300 ng/ml for cetirizine and ambroxol respectively in plasma and 1-500 ng/ml and 5-400 ng/ml, respectively for cetirizine and ambroxol in urine. Intra-day and inter-day precision of cetirizine and ambroxol was below 15% in terms of coefficient of variation and accuracy of cetirizine and ambroxol was ranged from 94 to 101.6% and 91.1 to 100.2%, respectively. The method demonstrated high sensitivity and selectivity and therefore, applied to evaluate pharmacokinetics of cetirizine and ambroxol in healthy human volunteer after a single oral administration. Urine samples obtained from healthy human volunteers and clinical subjects with renal impairment have also been analyzed by the method to compare the elimination pattern. The method was precise and accurate for the estimation of cetirizine and ambroxol both in blood and in urine. Copyright © 2011 Elsevier B.V. All rights reserved.

Spectrophotometric analyses of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in water.

PubMed

Shi, Cong; Xu, Zhonghou; Smolinski, Benjamin L; Arienti, Per M; O'Connor, Gregory; Meng, Xiaoguang

2015-07-01

A simple and accurate spectrophotometric method for on-site analysis of royal demolition explosive (RDX) in water samples was developed based on the Berthelot reaction. The sensitivity and accuracy of an existing spectrophotometric method was improved by: replacing toxic chemicals with more stable and safer reagents; optimizing the reagent dose and reaction time; improving color stability; and eliminating the interference from inorganic nitrogen compounds in water samples. Cation and anion exchange resin cartridges were developed and used for sample pretreatment to eliminate the effect of ammonia and nitrate on RDX analyses. The detection limit of the method was determined to be 100 μg/L. The method was used successfully for analysis of RDX in untreated industrial wastewater samples. It can be used for on-site monitoring of RDX in wastewater for early detection of chemical spills and failure of wastewater treatment systems. Copyright © 2015. Published by Elsevier B.V.

Quantitative bioanalysis of strontium in human serum by inductively coupled plasma-mass spectrometry

PubMed Central

Somarouthu, Srikanth; Ohh, Jayoung; Shaked, Jonathan; Cunico, Robert L; Yakatan, Gerald; Corritori, Suzana; Tami, Joe; Foehr, Erik D

2015-01-01

Aim: A bioanalytical method using inductively-coupled plasma-mass spectrometry to measure endogenous levels of strontium in human serum was developed and validated. Results & methodology: This article details the experimental procedures used for the method development and validation thus demonstrating the application of the inductively-coupled plasma-mass spectrometry method for quantification of strontium in human serum samples. The assay was validated for specificity, linearity, accuracy, precision, recovery and stability. Significant endogenous levels of strontium are present in human serum samples ranging from 19 to 96 ng/ml with a mean of 34.6 ± 15.2 ng/ml (SD). Discussion & conclusion: Calibration procedures and sample pretreatment were simplified for high throughput analysis. The validation demonstrates that the method was sensitive, selective for quantification of strontium (88Sr) and is suitable for routine clinical testing of strontium in human serum samples. PMID:28031925

Pretreatment of agricultural biomass for anaerobic digestion: Current state and challenges.

PubMed

Paudel, Shukra Raj; Banjara, Sushant Prasad; Choi, Oh Kyung; Park, Ki Young; Kim, Young Mo; Lee, Jae Woo

2017-12-01

The anaerobic digestion (AD) of agricultural biomass is an attractive second generation biofuel with potential environmental and economic benefits. Most agricultural biomass contains lignocellulose which requires pretreatment prior to AD. For optimization, the pretreatment methods need to be specific to the characteristics of the biomass feedstock. In this review, cereal residue, fruit and vegetable wastes, grasses and animal manure were selected as the agricultural biomass candidates, and the fundamentals and current state of various pretreatment methods used for AD of these feedstocks were investigated. Several nonconventional methods (electrical, ionic liquid-based chemicals, ruminant biological pretreatment) offer potential as targeted pretreatments of lignocellulosic biomass, but each comes with its own challenges. Pursuing an energy-intensive route, a combined bioethanol-biogas production could be a promising a second biofuel refinery option, further emphasizing the importance of pretreatment when lignocellulosic feedstock is used. Copyright © 2017 Elsevier Ltd. All rights reserved.

Research on identification and determination of mixed pesticides in apples using surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Zhai, Chen; Li, Yongyu; Peng, Yankun; Xu, Tianfeng; Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei

2015-05-01

Residual pesticides in fruits and vegetables have become one of the major food safety concerns around the world. At present, routine analytical methods used for the determination of pesticide residue on the surface of fruits and vegetables are destructive, complex, time-consuming, high cost and not environmentally friendly. In this study, a novel Surface Enhanced Raman Spectroscopy (SERS) method with silver colloid was developed for fast and sensitive nondestructive detection of residual pesticides in fruits and vegetables by using a self-developed Raman system. SERS technology is a combination of Raman spectroscopy and nanotechnology. SERS can greatly enhance the Raman signal intensity, achieve single-molecule detection, and has a simple sample pre-treatment characteristic of high sensitivity and no damage; in recent years it has begun to be used in food safety testing research. In this study a rapid and sensitive method was developed to identify and analyze mixed pesticides of chlorpyrifos, deltamethrin and acetamiprid in apple samples by SERS. Silver colloid was used for SERS measurement by hydroxylamine hydrochloride reduced. The advantages of this method are seen in its fast preparation at room temperature, good reproducibility and immediate applicability. Raman spectrum is highly interfered by noise signals and fluorescence background, which make it too complex to get good result. In this study the noise signals and fluorescence background were removed by Savitzky-Golay filter and min-max signal adaptive zooming method. Under optimal conditions, pesticide residues in apple samples can be detected by SERS at 0.005 μg/cm2 and 0.002 μg/cm2 for individual acetamiprid and thiram, respectively. When mixing the two pesticides at low concentrations, their characteristic peaks can still be identified from the SERS spectrum of the mixture. Based on the synthesized material and its application in SERS operation, the method represents an ultrasensitive SERS performance in apple samples detection without sample pre-treatment, which indicates that it could be served as a useful means in monitoring pesticide residues.

Electrochemical and/or microbiological treatment of pyrolysis wastewater.

PubMed

Silva, José R O; Santos, Dara S; Santos, Ubiratan R; Eguiluz, Katlin I B; Salazar-Banda, Giancarlo R; Schneider, Jaderson K; Krause, Laiza C; López, Jorge A; Hernández-Macedo, Maria L

2017-10-01

Electrochemical oxidation may be used as treatment to decompose partially or completely organic pollutants (wastewater) from industrial processes such as pyrolysis. Pyrolysis is a thermochemical process used to obtain bio-oil from biomasses, generating a liquid waste rich in organic compounds including aldehydes and phenols, which can be submitted to biological and electrochemical treatments in order to minimize its environmental impact. Thus, electrochemical systems employing dimensionally stable anodes (DSAs) have been proposed to enable biodegradation processes in subsurface environments. In order to investigate the organic compound degradation from residual coconut pyrolysis wastewater, ternary DSAs containing ruthenium, iridium and cerium synthetized by the 'ionic liquid method' at different calcination temperatures (500, 550, 600 and 700 °C) for the pretreatment of these compounds, were developed in order to allow posterior degradation by Pseudomonas sp., Bacillus sp. or Acinetobacter sp. bacteria. The electrode synthesized applying 500 °C displayed the highest voltammetric charge and was used in the pretreatment of pyrolysis effluent prior to microbial treatment. Regarding biological treatment, the Pseudomonas sp. exhibited high furfural degradation in wastewater samples electrochemically pretreated at 2.0 V. On the other hand, the use of Acinetobacter efficiently degraded phenolic compounds such as phenol, 4-methylphenol, 2,5-methylphenol, 4-ethylphenol and 3,5-methylphenol in both wastewater samples, with and without electrochemical pretreatment. Overall, the results indicate that the combination of both processes used in this study is relevant for the treatment of pyrolysis wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

Perform Tests and Document Results and Analysis of Oxide Layer Effects and Comparisons

DOE Office of Scientific and Technical Information (OSTI.GOV)

Collins, E. D.; DelCul, G. D.; Spencer, B. B.

2014-08-30

During the initial feasibility test using actual used nuclear fuel (UNF) cladding in FY 2012, an incubation period of 30–45 minutes was observed in the initial dry chlorination. The cladding hull used in the test had been previously oxidized in a dry air oxidation pretreatment prior to removal of the fuel. The cause of this incubation period was attributed to the resistance to chlorination of an oxide layer imparted by the dry oxidation pretreatment on the cladding. Subsequently in 2013, researchers at the Korea Atomic Energy Institute (KAERI) reported on their chlorination study [R1] on ~9-gram samples of unirradiated ZirloTMmore » cladding tubes that had been previously oxidized in air at 500oC for various time periods to impart oxide layers of varying thickness. In early 2014, discussions with Indefinite Delivery, Indefinite Quantity (IDIQ) contracted technical consultants from Westinghouse described their previous development (and patents) [R2] on methods of chemical washing to remove some or all of the hydrous oxide layer imparted on UNF cladding during irradiation in light water reactors (LWRs) . Thus, the Oak Ridge National Laboratory (ORNL) study, described herein, was planned to extend the KAERI study on the effects of anhydrous oxide layers, but on larger ~100-gram samples of unirradiated zirconium alloy cladding tubes, and to investigate the effects of various methods of chemical pretreatment prior to chlorination with 100% chlorine on the average reaction rates and Cl2 usage efficiencies.« less

Pretreatment of Biomass by Aqueous Ammonia for Bioethanol Production

NASA Astrophysics Data System (ADS)

Kim, Tae Hyun; Gupta, Rajesh; Lee, Y. Y.

The methods of pretreatment of lignocellulosic biomass using aqueous ammonia are described. The main effect of ammonia treatment of biomass is delignification without significantly affecting the carbohydrate contents. It is a very effective pretreatment method especially for substrates that have low lignin contents such as agricultural residues and herbaceous feedstock. The ammonia-based pretreatment is well suited for simultaneous saccharification and co-fermentation (SSCF) because the treated biomass retains cellulose as well as hemicellulose. It has been demonstrated that overall ethanol yield above 75% of the theoretical maximum on the basis of total carbohydrate is achievable from corn stover pretreated with aqueous ammonia by way of SSCF. There are two different types of pretreatment methods based on aqueous ammonia: (1) high severity, low contact time process (ammonia recycle percolation; ARP), (2) low severity, high treatment time process (soaking in aqueous ammonia; SAA). Both of these methods are described and discussed for their features and effectiveness.

Pretreatment of Cellulose By Electron Beam Irradiation Method

NASA Astrophysics Data System (ADS)

Jusri, N. A. A.; Azizan, A.; Ibrahim, N.; Salleh, R. Mohd; Rahman, M. F. Abd

2018-05-01

Pretreatment process of lignocellulosic biomass (LCB) to produce biofuel has been conducted by using various methods including physical, chemical, physicochemical as well as biological. The conversion of bioethanol process typically involves several steps which consist of pretreatment, hydrolysis, fermentation and separation. In this project, microcrystalline cellulose (MCC) was used in replacement of LCB since cellulose has the highest content of LCB for the purpose of investigating the effectiveness of new pretreatment method using radiation technology. Irradiation with different doses (100 kGy to 1000 kGy) was conducted by using electron beam accelerator equipment at Agensi Nuklear Malaysia. Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD) analyses were studied to further understand the effect of the suggested pretreatment step to the content of MCC. Through this method namely IRR-LCB, an ideal and optimal condition for pretreatment prior to the production of biofuel by using LCB may be introduced.

[Determination of Cu in Shell of Preserved Egg by LIBS Coupled with PLS].

PubMed

Hu, Hui-qin; Xu, Xue-hong; Liu, Mu-hua; Tu, Jian-ping; Huang, Le; Huang, Lin; Yao, Ming-yin; Chen, Tian-bing; Yang, Ping

2015-12-01

In this work, the content of copper in the shell of preserved eggs were determined directly by Laser induced breakdown spectroscopy (LIBS), and the characteristics lines of Cu was obtained. The samples of eggshell were pretreated by acid wet digestion, and the real content of Cu was obtained by atomic absorption spectrophotometer (AAS). Due to the test precision and accuracy of LIBS was influenced by a serious of factors, for example, the complex matrix effect of sample, the enviro nment noise, the system noise of the instrument, the stability of laser energy and so on. And the conventional unvariate linear calibration curve between LIBS intensity and content of element of sample, such as by use of Schiebe G-Lomakin equation, can not meet the requirement of quantitative analysis. In account of that, a kind of multivariate calibration method is needed. In this work, the data of LIBS spectra were processed by partial least squares (PLS), the precision and accuracy of PLS model were compared by different smoothing treatment and five pretreatment methods. The result showed that the correlation coefficient and the accuracy of the PLS model were improved, and the root mean square error and the average relative error were reduced effectively by 11 point smoothing with Multiplicative scatter correction (MSC) pretreatment. The results of the study show that, heavy metal Cu in preserved egg shells can be direct detected accurately by laser induced breakdown spectroscopy, and the next step batch tests will been conducted to find out the relationship of heavy metal Cu content in the preserved egg between the eggshell, egg white and egg yolk. And the goal of the contents of heavy metals in the egg white, egg yolk can be knew through determinate the eggshell by the LIBS can be achieved, to provide new method for rapid non-destructive testing technology for quality and satety of agricultural products.

Determination of glucose and ethanol after enzymatic hydrolysis and fermentation of biomass using Raman spectroscopy.

PubMed

Shih, Chien-Ju; Smith, Emily A

2009-10-27

Raman spectroscopy has been used for the quantitative determination of the conversion efficiency at each step in the production of ethanol from biomass. The method requires little sample preparation; therefore, it is suitable for screening large numbers of biomass samples and reaction conditions in a complex sample matrix. Dilute acid or ammonia-pretreated corn stover was used as a model biomass for these studies. Ammonia pretreatment was suitable for subsequent measurements with Raman spectroscopy, but dilute acid-pretreated corn stover generated a large background signal that surpassed the Raman signal. The background signal is attributed to lignin, which remains in the plant tissue after dilute acid pretreatment. A commercial enzyme mixture was used for the enzymatic hydrolysis of corn stover, and glucose levels were measured with a dispersive 785 nm Raman spectrometer. The glucose detection limit in hydrolysis liquor by Raman spectroscopy was 8 g L(-1). The mean hydrolysis efficiency for three replicate measurements obtained with Raman spectroscopy (86+/-4%) was compared to the result obtained using an enzymatic reaction with UV-vis spectrophotometry detection (78+/-8%). The results indicate good accuracy, as determined using a Student's t-test, and better precision for the Raman spectroscopy measurement relative to the enzymatic detection assay. The detection of glucose in hydrolysis broth by Raman spectroscopy showed no spectral interference, provided the sample was filtered to remove insoluble cellulose prior to analysis. The hydrolysate was further subjected to fermentation to yield ethanol. The detection limit for ethanol in fermentation broth by Raman spectroscopy was found to be 6 g L(-1). Comparison of the fermentation efficiencies measured by Raman spectroscopy (80+/-10%) and gas chromatography-mass spectrometry (87+/-9%) were statistically the same. The work demonstrates the utility of Raman spectroscopy for screening the entire conversion process to generate lignocellulosic ethanol.

Advances in the Diagnosis of Human Opisthorchiasis: Development of Opisthorchis viverrini Antigen Detection in Urine

PubMed Central

Duenngai, Kunyarat; Wangboon, Chompunoot; Sithithaworn, Jiraporn; Watwiengkam, Nattaya; Namwat, Nisana; Techasen, Anchalee; Loilome, Watcharin; Yongvanit, Puangrat; Loukas, Alex; Sithithaworn, Paiboon; Bethony, Jeffrey M.

2015-01-01

Background Many strategies to control opisthorchiasis have been employed in Thailand, but not in the other neighbouring countries. Specific control methods include mass drug administration (MDA) and health education to reduce raw fish consumption. These control efforts have greatly shifted the epidemiology of Opisthorchis viverrini (OV) infection over the last decade from presenting as densely concentrated "heavy" infections in single villages to widespread "light" OV infections distributed over wide geographical areas. Currently, the "gold standard" detection method for OV infection is formalin ethyl-acetate concentration technique (FECT), which has limited diagnostic sensitivity and diagnostic specificity for light OV infections, with OV eggs often confused with eggs of minute intestinal flukes (MIFs) in feces. In this study, we developed and evaluated the diagnostic performance of a monoclonal antibody-based enzyme-linked immunosorbent assay for the measurement of OV excretory-secretory (ES) antigens in urine (urine OV-ES assay) for the diagnosis of opisthorchiasis compared to the gold standard detection FECT method. Methodology We tested several methods for pre-treating urine samples prior to testing the diagnostic performance of the urine OV-ES assay. Using trichloroacetic acid (TCA) pre-treated urine, we compared detection and quantification of OV infection using the urine OV-ES assay versus FECT in OV-endemic areas in Northeastern Thailand. Receiver operating characteristic (ROC) curves were used to determine the diagnostic sensitivity and specificity of the urine OV-ES assay using TCA pre-treated urine, and to establish diagnostic positivity thresholds. The Positive Predictive Value as well as the likelihood of obtaining a positive test result (LR+) or a negative test result (LR-) were calculated for the established diagnostic positivity threshold. Diagnostic risks (Odds Ratios) were estimated using logistic regression. Results When urine samples were pre-treated with TCA prior to use in the urine OV-ES assay, the analytical sensitivity was significantly improved. Using TCA pre-treatment of urine, the urine OV-ES assay had a limit of detection (LoD) of 39 ng/ml compared to the LoD of 52 ng/mL reported for coprological antigen detection methods. Similarly, the urine OV-ES assay correlated significantly with intensity of OV infection as measured by FECT. The urine OV-ES assay was also able to detect 28 individuals as positive from the 63 (44.4%) individuals previously determined to be negative using FECT. The likelihood of a positive diagnosis of OV infection by urine OV-ES assay increased significantly with the intensity of OV infection as determined by FECT. With reference to FECT, the sensitivity and specificity of the urine OV-ES assay was 81% and 70%, respectively. Conclusion The detection of OV-infection by the urine OV-ES assay showed much greater diagnostic sensitivity and diagnostic specificity than the current "gold standard" FECT method for the detection and quantification of OV infection. Due to its ease-of-use, and noninvasive sample collection (urine), the urine OV-ES assay offers the potential to revolutionize the diagnosis of liver fluke infection and provide an effective tool for control and elimination of these tumorigenic parasites. PMID:26485024

Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

PubMed

Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

2008-11-20

Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

Study of Crystallinity Index (CrI) of Oil Palm Frond Pretreatment using Aqueous [EMIM][OAc] in a Closed System

NASA Astrophysics Data System (ADS)

Abu Darim, R.; Azizan, A.; Salihon, J.

2018-05-01

The objective of this preliminary study is to identify the Crystalinity Index (CrI) of Oil Palm Frond (OPF) pretreated with 40% concentration of 1-ethyl-3-methylimidazolium acetate ionic liquid ([EMIM][OAc]) in a closed system. The morphology and structural changes of the pretreated OPF were examined by using Fourier Transform Infrared Spectrometer (FTIR) and X-Ray Diffraction (XRD). The pretreatment process was carried out in triplicates by loading 40% of [EMIM][OAc] concentration with 10 wt% of OPF loading in the Bio-ionic liquid-reactor. The pretreatment process was conducted for 3 hours with working volume of 70 mL and temperature of 110°C. A Bio-ionic liquid reactor was purposely designed for the lignocellulosic pretreatment by using aqueous ionic liquid at high temperature (higher than boiling point of water). The CrI of OPF pretreated with 40% concentration of [EMM][OAc] in a closed system observed was 9% lower from the untreated OPF and the result showed significant difference with 95% confidence level. Further examination of the untreated and pretreated OPF by using XRD showed that the diffraction pattern of the pretreated OPF samples was decreasing compared to the untreated OPF. The characteristic of the FTIR spectra of the pretreated OPF showed the presence of the cellulose I and occurrence of amorphous cellulosic in the samples. The findings from this study are expected to improve knowledge on pretreatment of OPF by using aqueous [EMIM][OAc] as a green economically viable process for future renewable energy.

Lignocellulose nanofibers prepared by ionic liquid pretreatment and subsequent mechanical nanofibrillation of bagasse powder: Application to esterified bagasse/polypropylene composites.

PubMed

Ninomiya, Kazuaki; Abe, Megumi; Tsukegi, Takayuki; Kuroda, Kosuke; Tsuge, Yota; Ogino, Chiaki; Taki, Kentaro; Taima, Tetsuya; Saito, Joji; Kimizu, Mitsugu; Uzawa, Kiyoshi; Takahashi, Kenji

2018-02-15

In the present study, we examined the efficacy of choline acetate (ChOAc, a cholinium ionic liquid))-assisted pretreatment of bagasse powder for subsequent mechanical nanofibrillation to produce lignocellulose nanofibers. Bagasse sample with ChOAc pretreatment and subsequent nanofibrillation (ChOAc/NF-bagasse) was prepared and compared to untreated control bagasse sample (control bagasse), bagasse sample with nanofibrillation only (NF-bagasse) and with ChOAc pretreatment only (ChOAc-bagasse). The specific surface area was 0.83m 2 /g, 3.1m 2 /g, 6.3m 2 /g, and 32m 2 /g for the control bagasse, ChOAc-bagasse, NF-bagasse, and the ChOAc/NF-bagasse, respectively. Esterified bagasse/polypropylene composites were prepared using the bagasse samples. ChOAc/NF-bagasse exhibited the best dispersion in the composites. The tensile toughness of the composites was 0.52J/cm 3 , 0.73J/cm 3 , 0.92J/cm 3 , and 1.29J/cm 3 for the composites prepared using control bagasse, ChOAc-bagasse, NF-bagasse, and ChOAc/NF-bagasse, respectively. Therefore, ChOAc pretreatment and subsequent nanofibrillation of bagasse powder resulted in enhanced tensile toughness of esterified bagasse/polypropylene composites. Copyright © 2017 Elsevier Ltd. All rights reserved.

Long-term storage of salivary cortisol samples at room temperature

NASA Technical Reports Server (NTRS)

Chen, Yu-Ming; Cintron, Nitza M.; Whitson, Peggy A.

1992-01-01

Collection of saliva samples for the measurement of cortisol during space flights provides a simple technique for studying changes in adrenal function due microgravity. In the present work, several methods for preserving saliva cortisol at room temperature were investigated using radioimmunoassays for determining cortisol in saliva samples collected on a saliva-collection device called Salivettes. It was found that a pretreatment of Salivettes with citric acid resulted in preserving more than 85 percent of the salivary cortisol for as long as six weeks. The results correlated well with those for a sample stored in a freezer on an untreated Salivette.

A novel hybrid organosolv: steam explosion method for the efficient fractionation and pretreatment of birch biomass.

PubMed

Matsakas, Leonidas; Nitsos, Christos; Raghavendran, Vijayendran; Yakimenko, Olga; Persson, Gustav; Olsson, Eva; Rova, Ulrika; Olsson, Lisbeth; Christakopoulos, Paul

2018-01-01

The main role of pretreatment is to reduce the natural biomass recalcitrance and thus enhance saccharification yield. A further prerequisite for efficient utilization of all biomass components is their efficient fractionation into well-defined process streams. Currently available pretreatment methods only partially fulfill these criteria. Steam explosion, for example, excels as a pretreatment method but has limited potential for fractionation, whereas organosolv is excellent for delignification but offers poor biomass deconstruction. In this article, a hybrid method combining the cooking and fractionation of conventional organosolv pretreatment with the implementation of an explosive discharge of the cooking mixture at the end of pretreatment was developed. The effects of various pretreatment parameters (ethanol content, duration, and addition of sulfuric acid) were evaluated. Pretreatment of birch at 200 °C with 60% v/v ethanol and 1% w/w biomass H 2 SO 4 was proven to be the most efficient pretreatment condition yielding pretreated solids with 77.9% w/w cellulose, 8.9% w/w hemicellulose, and 7.0 w/w lignin content. Under these conditions, high delignification of 86.2% was demonstrated. The recovered lignin was of high purity, with cellulose and hemicellulose contents not exceeding 0.31 and 3.25% w/w, respectively, and ash to be < 0.17% w/w in all cases, making it suitable for various applications. The pretreated solids presented high saccharification yields, reaching 68% at low enzyme load (6 FPU/g) and complete saccharification at high enzyme load (22.5 FPU/g). Finally, simultaneous saccharification and fermentation (SSF) at 20% w/w solids yielded an ethanol titer of 80 g/L after 192 h, corresponding to 90% of the theoretical maximum. The novel hybrid method developed in this study allowed for the efficient fractionation of birch biomass and production of pretreated solids with high cellulose and low lignin contents. Moreover, the explosive discharge at the end of pretreatment had a positive effect on enzymatic saccharification, resulting in high hydrolyzability of the pretreated solids and elevated ethanol titers in the following high-gravity SSF. To the best of our knowledge, the ethanol concentration obtained with this method is the highest so far for birch biomass.

Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

PubMed

Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

2017-09-15

This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

Pretreatment of microbial sludges

DOEpatents

Rivard, Christopher J.; Nagle, Nicholas J.

1995-01-01

Methods are described for pretreating microbial sludges to break cells and disrupt organic matter. One method involves the use of sonication, and another method involves the use of shear forces. The pretreatment of sludge enhances bioconversion of the organic fraction. This allows for efficient dewatering of the sludge and reduces the cost for final disposal of the waste.

Pretreatment of microbial sludges

DOEpatents

Rivard, C.J.; Nagle, N.J.

1995-01-10

Methods are described for pretreating microbial sludges to break cells and disrupt organic matter. One method involves the use of sonication, and another method involves the use of shear forces. The pretreatment of sludge enhances bioconversion of the organic fraction. This allows for efficient dewatering of the sludge and reduces the cost for final disposal of the waste.

Quantifications of dendrochronological information from contrasting microdensitometric measuring circumstances of experimental wood samples.

PubMed

Helama, S; Bégin, Y; Vartiainen, M; Peltola, H; Kolström, T; Meriläinen, J

2012-06-01

We analyzed how the pretreatment method of Scots pine (Pinus sylvestris L.) wood specimens together with X-ray methodology applied for density analyses affect resulting tree-ring data and derived proxy-based climate information. We also evaluated whether these results from two contrasting laboratory circumstances could be homogenized by applying dendroclimatic statistical methods. For this study, we measured a pair of X-ray based microdensitometry datasets using double samples of subfossil and recent wood specimens. Dendrochronological information of earlywood and latewood series was examined to determine for alterations in the resulting data. We found that the level of overall density, its trend over cambial ages and the growth amplitude altered due to the sample pretreatment/density measuring exercise, which means that comparisons of heterogeneous datasets should be, in general, regarded cautiously. Dendrochronological standardization did, however, even out several potentially biasing influences from the differing overall densities and their trends. The two latewood (maximum) density chronologies yielded paleoclimatic reconstructions which both calibrated and verified satisfactorily with the instrumental warm-season (March-September) mean temperatures. The transfer functions were found to further equalize the differences between the two proxy records. We recommend (if no strictly homogenous data are available) reconciling similar data assemblages through transfer functions with multiple independent variables. Copyright © 2012 Elsevier Ltd. All rights reserved.

Comparative evaluation of hepatitis C virus RNA quantitation by branched DNA, NASBA, and monitor assays.

PubMed

Lunel, F; Cresta, P; Vitour, D; Payan, C; Dumont, B; Frangeul, L; Reboul, D; Brault, C; Piette, J C; Huraux, J M

1999-02-01

Several studies have shown a relationship between pretreatment hepatitis C virus (HCV) viral load and the response to interferon (IFN) therapy, creating a need for quantitative HCV-RNA assays. Here, we compared three commercial methods: nucleic acid sequence-based amplification NASBA (Organon), branched DNA 2.0 (bDNA) (Chiron), and Monitor (Roche), with reverse-transcription polymerase chain reaction (RT-PCR) as the reference. We assessed sensitivity and reproducibility on a well-characterized panel of sera (EUROHEP), a Chimp Rodney plasma pool, and samples from IFN-treated and -untreated patients with chronic hepatitis C caused by different HCV genotypes. The reproducibility of the NASBA and bDNA methods was slightly better than that of Monitor, especially for genotypes 2 and 4. NASBA had the highest sensitivity (99% vs. 94% and 88% with Monitor and bDNA, respectively), especially for the follow-up of patients on IFN. NASBA gave the highest HCV-RNA concentrations, which were approximately 10-fold more than with the bDNA assay and 100-fold more than with the Monitor kit. The linearity, tested on the chimp Rodney plasma pool, was better with bDNA for high viral load than with NASBA and Monitor, although for low concentration of HCV RNA, bDNA was negative. Pretreatment viral load was lower in patients who had a sustained virological response to IFN, although the bDNA method was not sensitive enough to quantify all pretreatment samples. This study indicates that gene amplification methods (NASBA or Monitor) have better sensitivity than bDNA assays for quantification of HCV RNA in patients with chronic HCV infection, although the bDNA and NASBA methods are more likely to quantify all genotypes. Prospective studies are needed to demonstrate the usefulness of quantitative assays for the follow-up of patients with chronic hepatitis C.

Improved sugar yields from biomass sorghum feedstocks: comparing low-lignin mutants and pretreatment chemistries.

PubMed

Godin, Bruno; Nagle, Nick; Sattler, Scott; Agneessens, Richard; Delcarte, Jérôme; Wolfrum, Edward

2016-01-01

For biofuel production processes to be economically efficient, it is essential to maximize the production of monomeric carbohydrates from the structural carbohydrates of feedstocks. One strategy for maximizing carbohydrate production is to identify less recalcitrant feedstock cultivars by performing some type of experimental screening on a large and diverse set of candidate materials, or by identifying genetic modifications (random or directed mutations or transgenic plants) that provide decreased recalcitrance. Economic efficiency can also be increased using additional pretreatment processes such as deacetylation, which uses dilute NaOH to remove the acetyl groups of hemicellulose prior to dilute acid pretreatment. In this work, we used a laboratory-scale screening tool that mimics relevant thermochemical pretreatment conditions to compare the total sugar yield of three near-isogenic brown midrib ( bmr ) mutant lines and the wild-type (WT) sorghum cultivar. We then compared results obtained from the laboratory-scale screening pretreatment assay to a large-scale pretreatment system. After pretreatment and enzymatic hydrolysis, the bmr mutants had higher total sugar yields than the WT sorghum cultivar. Increased pretreatment temperatures increased reactivity for all sorghum samples reducing the differences observed at lower reaction temperatures. Deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples, and reduced the differences in total sugar yields among them, but solubilized a sizable fraction of the non-structural carbohydrates. The general trends of increased total sugar yield in the bmr mutant compared to the WT seen at the laboratory scale were observed at the large-scale system. However, in the larger reactor system, the measured total sugar yields were lower and the difference in total sugar yield between the WT and bmr sorghum was larger. Sorghum bmr mutants, which have a reduced lignin content showed higher total sugar yields than the WT cultivar after dilute acid pretreatment and enzymatic hydrolysis. Deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples. However, since deacetylation also solubilizes a large fraction of the non-structural carbohydrates, the ability to derive value from these solubilized sugars will depend greatly on the proposed conversion process.

Improved sugar yields from biomass sorghum feedstocks: comparing low-lignin mutants and pretreatment chemistries

DOE PAGES

Godin, Bruno; Nagle, Nick; Sattler, Scott; ...

2016-11-21

For biofuel production processes to be economically efficient, it is essential to maximize the production of monomeric carbohydrates from the structural carbohydrates of feedstocks. One strategy for maximizing carbohydrate production is to identify less recalcitrant feedstock cultivars by performing some type of experimental screening on a large and diverse set of candidate materials, or by identifying genetic modifications (random or directed mutations or transgenic plants) that provide decreased recalcitrance. Economic efficiency can also be increased using additional pretreatment processes such as deacetylation, which uses dilute NaOH to remove the acetyl groups of hemicellulose prior to dilute acid pretreatment. In thismore » work, we used a laboratory-scale screening tool that mimics relevant thermochemical pretreatment conditions to compare the total sugar yield of three near-isogenic brown midrib (bmr) mutant lines and the wild-type (WT) sorghum cultivar. We then compared results obtained from the laboratory-scale screening pretreatment assay to a large-scale pretreatment system. After pretreatment and enzymatic hydrolysis, the bmr mutants had higher total sugar yields than the WT sorghum cultivar. Increased pretreatment temperatures increased reactivity for all sorghum samples reducing the differences observed at lower reaction temperatures. Deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples, and reduced the differences in total sugar yields among them, but solubilized a sizable fraction of the non-structural carbohydrates. The general trends of increased total sugar yield in the bmr mutant compared to the WT seen at the laboratory scale were observed at the large-scale system. However, in the larger reactor system, the measured total sugar yields were lower and the difference in total sugar yield between the WT and bmr sorghum was larger. Sorghum bmr mutants, which have a reduced lignin content showed higher total sugar yields than the WT cultivar after dilute acid pretreatment and enzymatic hydrolysis. In conclusion, deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples. However, since deacetylation also solubilizes a large fraction of the non-structural carbohydrates, the ability to derive value from these solubilized sugars will depend greatly on the proposed conversion process.« less

Improved sugar yields from biomass sorghum feedstocks: comparing low-lignin mutants and pretreatment chemistries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Godin, Bruno; Nagle, Nick; Sattler, Scott

For biofuel production processes to be economically efficient, it is essential to maximize the production of monomeric carbohydrates from the structural carbohydrates of feedstocks. One strategy for maximizing carbohydrate production is to identify less recalcitrant feedstock cultivars by performing some type of experimental screening on a large and diverse set of candidate materials, or by identifying genetic modifications (random or directed mutations or transgenic plants) that provide decreased recalcitrance. Economic efficiency can also be increased using additional pretreatment processes such as deacetylation, which uses dilute NaOH to remove the acetyl groups of hemicellulose prior to dilute acid pretreatment. In thismore » work, we used a laboratory-scale screening tool that mimics relevant thermochemical pretreatment conditions to compare the total sugar yield of three near-isogenic brown midrib (bmr) mutant lines and the wild-type (WT) sorghum cultivar. We then compared results obtained from the laboratory-scale screening pretreatment assay to a large-scale pretreatment system. After pretreatment and enzymatic hydrolysis, the bmr mutants had higher total sugar yields than the WT sorghum cultivar. Increased pretreatment temperatures increased reactivity for all sorghum samples reducing the differences observed at lower reaction temperatures. Deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples, and reduced the differences in total sugar yields among them, but solubilized a sizable fraction of the non-structural carbohydrates. The general trends of increased total sugar yield in the bmr mutant compared to the WT seen at the laboratory scale were observed at the large-scale system. However, in the larger reactor system, the measured total sugar yields were lower and the difference in total sugar yield between the WT and bmr sorghum was larger. Sorghum bmr mutants, which have a reduced lignin content showed higher total sugar yields than the WT cultivar after dilute acid pretreatment and enzymatic hydrolysis. In conclusion, deacetylation prior to dilute acid pretreatment increased the total sugar yield for all four sorghum samples. However, since deacetylation also solubilizes a large fraction of the non-structural carbohydrates, the ability to derive value from these solubilized sugars will depend greatly on the proposed conversion process.« less

Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

PubMed

Piñeiro, Zulema; Marrufo-Curtido, Almudena; Serrano, Maria Jose; Palma, Miguel

2016-06-16

An analytical ultrasound-assisted extraction (UAE) method has been optimized and validated for the rapid extraction of stilbenes from grape canes. The influence of sample pre-treatment (oven or freeze-drying) and several extraction variables (solvent, sample-solvent ratio and extraction time between others) on the extraction process were analyzed. The new method allowed the main stilbenes in grape canes to be extracted in just 10 min, with an extraction temperature of 75 °C and 60% ethanol in water as the extraction solvent. Validation of the extraction method was based on analytical properties. The resulting RSDs (n = 5) for interday/intraday precision were less than 10%. Furthermore, the method was successfully applied in the analysis of 20 different grape cane samples. The result showed that grape cane byproducts are potentially sources of bioactive compounds of interest for pharmaceutical and food industries.

[Rapid determination of the components in ternary blended edible oil using near infrared transmission spectroscopy].

PubMed

Liu, Fu-Li; Chen, Hua-Cai

2009-08-01

The FT-NIR transmission spectra of ternary blended edible oil samples were collected over 10 000-4 200 cm(-1). After being pretreated with different methods, the calibration models of quantitative analysis of soybean oil, peanut oil and corn oil contents in ternary blended edible oil were established using partial least square (PLS) regression. The accuracy and precision of the models for the predicted sample set were examined to make sure of the practicability of the models. After being pretreated with first derivative and multiplicative signal correction (FD+MSC), the optimal soybean oil NIR model was built over 5 450.1-4 597.7 cm(-1). The best prediction model for peanut oil was established between 7 521.3 and 6 098.1 cm(-1) after using first derivative with straight line subtraction (FD+SLS) preprocess method. The best pretreated method and the best spectrum range for corn oil content model were first derivative (FD) and 9 993.7-7 498.2 cm(-1), respectively. The best correlation coefficients (R2) of the three prediction models were 99.89%, 99.88% and 99.76%, respectively. The RMSEP of the soybean oil content model was 1.09%, while the peanut oil prediction model's RMSEP was 1.17%, and 1.48% for the corn oil prediction model. The values of the t-test were between 0.007 9 and 0.371 9, and all values of the relative standard deviation (RSD) were less than 1.50%. The results showed that NIR could be an ideal tool for fast determination of the soybean oil, peanut oil and corn oil contents in ternary blended edible oil.

Viral persistence in surface and drinking water: Suitability of PCR pre-treatment with intercalating dyes.

PubMed

Prevost, B; Goulet, M; Lucas, F S; Joyeux, M; Moulin, L; Wurtzer, S

2016-03-15

After many outbreaks of enteric virus associated with consumption of drinking water, the study of enteric viruses in water has increased significantly in recent years. In order to better understand the dynamics of enteric viruses in environmental water and the associated viral risk, it is necessary to estimate viral persistence in different conditions. In this study, two representative models of human enteric viruses, adenovirus 41 (AdV 41) and coxsackievirus B2 (CV-B2), were used to evaluate the persistence of enteric viruses in environmental water. The persistence of infectious particles, encapsidated genomes and free nucleic acids of AdV 41 and CV-B2 was evaluated in drinking water and surface water at different temperatures (4 °C, 20 °C and 37 °C). The infectivity of AdV 41 and CV-B2 persisted for at least 25 days, whatever the water temperature, and for more than 70 days at 4 °C and 20 °C, in both drinking and surface water. Encapsidated genomes persisted beyond 70 days, whatever the water temperature. Free nucleic acids (i.e. without capsid) also were able to persist for at least 16 days in drinking and surface water. The usefulness of a detection method based on an intercalating dye pre-treatment, which specifically targets preserved particles, was investigated for the discrimination of free and encapsidated genomes and it was compared to virus infectivity. Further, the resistance of AdV 41 and CV-B2 against two major disinfection treatments applied in drinking water plants (UV and chlorination) was evaluated. Even after the application of UV rays and chlorine at high doses (400 mJ/cm(2) and 10 mg.min/L, respectively), viral genomes were still detected with molecular biology methods. Although the intercalating dye pre-treatment had little use for the detection of the effects of UV treatment, it was useful in the case of treatment by chlorination and less than 1 log10 difference in the results was found as compared to the infectivity measurements. Finally, for the first time, the suitability of intercalating dye pre-treatment for the estimation of the quality of the water produced by treatment plants was demonstrated using samples from four drinking-water plants and two rivers. Although 55% (27/49) of drinking water samples were positive for enteric viruses using molecular detection, none of the samples were positive when the intercalating dye pre-treatment method was used. This could indicate that the viruses that were detected are not infectious. Copyright © 2016 Elsevier Ltd. All rights reserved.

Supercritical CO2 and ionic liquids for the pretreatment of lignocellulosic biomass in bioethanol production.

PubMed

Gu, Tingyue; Held, Michael A; Faik, Ahmed

2013-01-01

Owing to high petroleum prices, there has been a major push in recent years to use lignocellulosic biomass as biorefinery feedstocks. Unfortunately, by nature's design, lignocellulosic biomass is notoriously recalcitrant. Cellulose is the most abundant renewable carbon source on the planet and comprises glucan polysaccharides which self-assemble into paracrystalline microfibrils. The extent of cellulose crystallinity largely contributes to biomass recalcitrance. Additionally, cellulose microfibrils are embedded into both hemicellulose and lignin polymeric networks, making cellulose accessibility an additional obstacle. Pretreatment is necessary before enzymatic hydrolysis in order to liberate high yields of glucose and other fermentable sugars from biomass polysaccharides. This work discusses two pretreatment methods, supercritical CO2 and ionic liquids (ILs). Both methods utilize green solvents that do not emit toxic vapours. Mechanisms for destroying or weakening biomass recalcitrance have been explored. Various pretreatment operating parameters such as temperature, pressure, time, dry biomass/solvent ratio, water content, etc. have been investigated for the pretreatment of various biomass types such as corn stover, switchgrass, sugarcane bagasse, soft and hard wood. The two pretreatment methods have their pros and cons. For example, supercritical CO2 explosion pretreatment uses inexpensive CO2, but requires a high pressure. By comparison, while IL pretreatment does not require an elevated pressure, ILs are still too expensive for large-scale uses. Further research and development are needed to make the two green pretreatment methods practical.

Gender and Batterer Intervention: Implications of a Program Evaluation for Policy and Treatment

ERIC Educational Resources Information Center

Hamel, John; Ferreira, Regardt J.; Buttell, Fred

2017-01-01

Objective: The purpose of the present study was to investigate the impact of gender and other variables commonly associated with intimate partner abuse perpetration on program completion and pretreatment abusiveness profiles among a sample of men and women ordered into a 52-week batterer intervention program (BIP). Method: The study employed a…

RAPID METHOD FOR DETERMINATION OF RADIOSTRONTIUM IN EMERGENCY MILK SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.; Culligan, B.

2008-07-17

A new rapid separation method for radiostrontium in emergency milk samples was developed at the Savannah River Site (SRS) Environmental Bioassay Laboratory (Aiken, SC, USA) that will allow rapid separation and measurement of Sr-90 within 8 hours. The new method uses calcium phosphate precipitation, nitric acid dissolution of the precipitate to coagulate residual fat/proteins and a rapid strontium separation using Sr Resin (Eichrom Technologies, Darien, IL, USA) with vacuum-assisted flow rates. The method is much faster than previous method that use calcination or cation exchange pretreatment, has excellent chemical recovery, and effectively removes beta interferences. When a 100 ml samplemore » aliquot is used, the method has a detection limit of 0.5 Bq/L, well below generic emergency action levels.« less

Lignin content in natural Populus variants affects sugar release

PubMed Central

Studer, Michael H.; DeMartini, Jaclyn D.; Davis, Mark F.; Sykes, Robert W.; Davison, Brian; Keller, Martin; Tuskan, Gerald A.; Wyman, Charles E.

2011-01-01

The primary obstacle to producing renewable fuels from lignocellulosic biomass is a plant's recalcitrance to releasing sugars bound in the cell wall. From a sample set of wood cores representing 1,100 individual undomesticated Populus trichocarpa trees, 47 extreme phenotypes were selected across measured lignin content and ratio of syringyl and guaiacyl units (S/G ratio). This subset was tested for total sugar release through enzymatic hydrolysis alone as well as through combined hot-water pretreatment and enzymatic hydrolysis using a high-throughput screening method. The total amount of glucan and xylan released varied widely among samples, with total sugar yields of up to 92% of the theoretical maximum. A strong negative correlation between sugar release and lignin content was only found for pretreated samples with an S/G ratio < 2.0. For higher S/G ratios, sugar release was generally higher, and the negative influence of lignin was less pronounced. When examined separately, only glucose release was correlated with lignin content and S/G ratio in this manner, whereas xylose release depended on the S/G ratio alone. For enzymatic hydrolysis without pretreatment, sugar release increased significantly with decreasing lignin content below 20%, irrespective of the S/G ratio. Furthermore, certain samples featuring average lignin content and S/G ratios exhibited exceptional sugar release. These facts suggest that factors beyond lignin and S/G ratio influence recalcitrance to sugar release and point to a critical need for deeper understanding of cell-wall structure before plants can be rationally engineered for reduced recalcitrance and efficient biofuels production. PMID:21444820

Determination of low (137)Cs concentration in seawater using ammonium 12-molybdophosphate adsorption and chemical separation method.

PubMed

Park, J H; Chang, B U; Kim, Y J; Seo, J S; Choi, S W; Yun, J Y

2008-12-01

A new method has been developed for analyzing (137)Cs in a small volume of seawater. Ammonium 12-molybdophosphate (AMP) was used two times during pretreatment procedure. The first step was to adsorb (137)Cs in seawater samples into AMP in order to reduce sample volume, and the second was to remove (87)Rb, interference nuclide for beta counting. The AMP adsorbing (137)Cs was dissolved by sodium hydroxide solution, and then (137)Cs was finally formed to be cesium chloroplatinate precipitate by adding 10% hexachloroplatinic acid. The beta rays emitted from (137)Cs were measured with a low background gas-proportional alpha/beta counter. This method was applied to several seawater samples taken in the East Sea of Korea. Compared to the routinely used gamma-spectrometry method, this new AMP method was reliable and suitable for analyzing (137)Cs in deep seawater.

Influence of combined pretreatments on color parameters during convective drying of Mirabelle plum ( Prunus domestica subsp. syriaca)

NASA Astrophysics Data System (ADS)

Dehghannya, Jalal; Gorbani, Rasoul; Ghanbarzadeh, Babak

2017-07-01

Discoloration and browning are caused primarily by various reactions, including Maillard condensation of hexoses and amino components, phenol polymerization and pigment destruction. Convective drying can be combined with various pretreatments to help reduce undesired color changes and improve color parameters of dried products. In this study, effects of ultrasound-assisted osmotic dehydration as a pretreatment before convective drying on color parameters of Mirabelle plum were investigated. Variations of L* (lightness), a* (redness/greenness), b* (yellowness/blueness), total color change (ΔE), chroma, hue angle and browning index values were presented versus drying time during convective drying of control and pretreated Mirabelle plums as influenced by ultrasonication time, osmotic solution concentration and immersion time in osmotic solution. Samples pretreated with ultrasound for 30 min and osmotic solution concentration of 70% had a more desirable color among all other pretreated samples, with the closest L*, a* and b* values to the fresh one, showing that ultrasound and osmotic dehydration are beneficial to the color of final products after drying.

Sensitive, accurate and rapid detection of trace aliphatic amines in environmental samples with ultrasonic-assisted derivatization microextraction using a new fluorescent reagent for high performance liquid chromatography.

PubMed

Chen, Guang; Liu, Jianjun; Liu, Mengge; Li, Guoliang; Sun, Zhiwei; Zhang, Shijuan; Song, Cuihua; Wang, Hua; Suo, Yourui; You, Jinmao

2014-07-25

A new fluorescent reagent, 1-(1H-imidazol-1-yl)-2-(2-phenyl-1H-phenanthro[9,10-d]imidazol-1-yl)ethanone (IPPIE), is synthesized, and a simple pretreatment based on ultrasonic-assisted derivatization microextraction (UDME) with IPPIE is proposed for the selective derivatization of 12 aliphatic amines (C1: methylamine-C12: dodecylamine) in complex matrix samples (irrigation water, river water, waste water, cultivated soil, riverbank soil and riverbed soil). Under the optimal experimental conditions (solvent: ACN-HCl, catalyst: none, molar ratio: 4.3, time: 8 min and temperature: 80°C), micro amount of sample (40 μL; 5mg) can be pretreated in only 10 min, with no preconcentration, evaporation or other additional manual operations required. The interfering substances (aromatic amines, aliphatic alcohols and phenols) get the derivatization yields of <5%, causing insignificant matrix effects (<4%). IPPIE-analyte derivatives are separated by high performance liquid chromatography (HPLC) and quantified by fluorescence detection (FD). The very low instrumental detection limits (IDL: 0.66-4.02 ng/L) and method detection limits (MDL: 0.04-0.33 ng/g; 5.96-45.61 ng/L) are achieved. Analytes are further identified from adjacent peaks by on-line ion trap mass spectrometry (MS), thereby avoiding additional operations for impurities. With this UDME-HPLC-FD-MS method, the accuracy (-0.73-2.12%), precision (intra-day: 0.87-3.39%; inter-day: 0.16-4.12%), recovery (97.01-104.10%) and sensitivity were significantly improved. Successful applications in environmental samples demonstrate the superiority of this method in the sensitive, accurate and rapid determination of trace aliphatic amines in micro amount of complex samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Influence of amino acids Shiff bases on irradiated DNA stability in vivo.

PubMed

Karapetyan, N H; Malakyan, M H; Bajinyan, S A; Torosyan, A L; Grigoryan, I E; Haroutiunian, S G

2013-01-01

To reveal protective role of the new Mn(II) complexes with Nicotinyl-L-Tyrosinate and Nicotinyl-L-Tryptophanate Schiff Bases against ionizing radiation. The DNA of the rats liver was isolated on 7, 14, and 30 days after X-ray irradiation. The differences between the DNA of irradiated rats and rats pre-treated with Mn(II) complexes were studied using the melting, microcalorimetry, and electrophoresis methods. The melting parameters and the melting enthalpy of rats livers DNA were changed after the X-ray irradiation: melting temperature and melting enthalpy were decreased and melting interval was increased. These results can be explained by destruction of DNA molecules. It was shown that pre-treatment of rats with Mn(II) complexes approximates the melting parameters to norm. Agarose gel electrophoresis data confirmed the results of melting studies. The separate DNA fragments were revealed in DNA samples isolated from irradiated animals. The DNA isolated from animals pre-treated with the Mn(II) chelates had better electrophoretic characteristics, which correspond to healthy DNA. Pre-treatment of the irradiated rats with Mn(II)(Nicotinil-L-Tyrosinate) and Mn(II)(Nicotinil-L-Tryptophanate)2 improves the DNA characteristics.

Effect of high carbon dioxide atmosphere packaging and soluble gas stabilization pre-treatment on the shelf-life and quality of chicken drumsticks.

PubMed

Al-Nehlawi, A; Saldo, J; Vega, L F; Guri, S

2013-05-01

The effects of an aerobic modified atmosphere packaging (MAP) (70% CO2, 15% O2 and 15% N2) with and without a CO2 3-h soluble gas stabilization (SGS) pre-treatment of chicken drumsticks were determined for various package and product quality characteristics. The CO2 dissolved into drumsticks was determined. The equilibrium between CO2 dissolved in drumsticks and CO2 in head space was reached within 48h after packaging, showing highest values of CO2 in SGS pre-treated samples. This greater availability of CO2 resulted in lower counts of TAB and Pseudomonas in SGS than in MAP drumsticks. Package collapse was significantly reduced in SGS samples. The average of CO2 dissolved in the MAP treatment was 567mg CO2kg(-1) of chicken and, 361mg CO2kg(-1) of chicken during the MAP treatment, in SGS pre-treated samples. This difference could be the quantity of CO2 dissolved during SGS pre-treatment. These results highlight the advantages of using SGS versus traditional MAP for chicken products preservation. Copyright © 2013 Elsevier Ltd. All rights reserved.

ECLSS Sustaining Compatibility Testing on Urine Processor Assembly Nonmetallic Materials for Reformulation of Pretreated Urine Solution

NASA Technical Reports Server (NTRS)

Wingard, C. D.

2015-01-01

On International Space Station (ISS), the Urine Processor Assembly (UPA) converts human urine and flush water into potable water. The urine is acid-pretreated primarily to control microbial growth. In recent years, the sulfuric acid (H2SO4) pretreatment was believed to be largely responsible for producing salt crystals capable of plugging filters in UPA components and significantly reducing the percentage of water recovery from urine. In 2012, ISS management decided to change the acid pretreatment for urine from sulfuric to phosphoric with the goal of eliminating or minimizing formation of salt crystals. In 2013-2014, as part of the qualification of the phosphoric acid (H3PO4) formulation, samples of 12 nonmetallic materials used in UPA components were immersed for up to one year in pretreated urine and brine solutions made with the new H3PO4 formulation. Dynamic mechanical analysis (DMA) was used to measure modulus (stiffness) of the immersed samples compared to virgin control samples. Such compatibility data obtained by DMA for the H3PO4-based solutions were compared to DMA data obtained for the H2SO4-based solutions in 2002-2003.

Ultrasound assisted biogas production from landfill leachate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oz, Nilgün Ayman, E-mail: nilgunayman@comu.edu.tr; Yarimtepe, Canan Can

Highlights: • Effect of low frequency ultrasound pretreatment on leachate was investigated. • Three different ultrasound energy inputs (200, 400 and 600 W/l) was applied. • Low-frequency ultrasound treatment increased soluble COD in landfill leachate. • Application of ultrasound to leachate increased biogas production about 40%. • Application of ultrasound to leachate increased total methane production rate about 20%. - Abstract: The aim of this study is to increase biogas production and methane yield from landfill leachate in anaerobic batch reactors by using low frequency ultrasound as a pretreatment step. In the first part of the study, optimum conditions formore » solubilization of organic matter in leachate samples were investigated using various sonication durations at an ultrasound frequency of 20 kHz. The level of organic matter solubilization during ultrasonic pretreatment experiments was determined by calculating the ratio of soluble chemical oxygen demand (sCOD) to total chemical oxygen demand (tCOD). The sCOD/tCOD ratio was increased from 47% in raw leachate to 63% after 45 min sonication at 600 W/l. Non-parametric Friedman’s test indicated that ultrasonic pretreatment has a significant effect on sCOD parameter for leachate (p < 0.05). In the second part of the study, anaerobic batch reactors were operated for both ultrasonically pretreated and untreated landfill leachate samples in order to assess the effect of sonication on biogas and methane production rate. In anaerobic batch reactor feed with ultrasonically pretreated leachate, 40% more biogas was obtained compared to the control reactor. For statistical analysis, Mann–Whitney U test was performed to compare biogas and methane production rates for raw and pretreated leachate samples and it has been found that ultrasonic pretreatment significantly enhanced biogas and methane production rates from leachate (p < 0.05) in anaerobic batch reactors. The overall results showed that low frequency ultrasound pretreatment can be potentially used for wastewater management especially with integration of anaerobic processes.« less

[Main Components of Xinjiang Lavender Essential Oil Determined by Partial Least Squares and Near Infrared Spectroscopy].

PubMed

Liao, Xiang; Wang, Qing; Fu, Ji-hong; Tang, Jun

2015-09-01

This work was undertaken to establish a quantitative analysis model which can rapid determinate the content of linalool, linalyl acetate of Xinjiang lavender essential oil. Totally 165 lavender essential oil samples were measured by using near infrared absorption spectrum (NIR), after analyzing the near infrared spectral absorption peaks of all samples, lavender essential oil have abundant chemical information and the interference of random noise may be relatively low on the spectral intervals of 7100~4500 cm(-1). Thus, the PLS models was constructed by using this interval for further analysis. 8 abnormal samples were eliminated. Through the clustering method, 157 lavender essential oil samples were divided into 105 calibration set samples and 52 validation set samples. Gas chromatography mass spectrometry (GC-MS) was used as a tool to determine the content of linalool and linalyl acetate in lavender essential oil. Then the matrix was established with the GC-MS raw data of two compounds in combination with the original NIR data. In order to optimize the model, different pretreatment methods were used to preprocess the raw NIR spectral to contrast the spectral filtering effect, after analysizing the quantitative model results of linalool and linalyl acetate, the root mean square error prediction (RMSEP) of orthogonal signal transformation (OSC) was 0.226, 0.558, spectrally, it was the optimum pretreatment method. In addition, forward interval partial least squares (FiPLS) method was used to exclude the wavelength points which has nothing to do with determination composition or present nonlinear correlation, finally 8 spectral intervals totally 160 wavelength points were obtained as the dataset. Combining the data sets which have optimized by OSC-FiPLS with partial least squares (PLS) to establish a rapid quantitative analysis model for determining the content of linalool and linalyl acetate in Xinjiang lavender essential oil, numbers of hidden variables of two components were 8 in the model. The performance of the model was evaluated according to root mean square error of cross-validation (RMSECV), root mean square error of prediction (RMSEP). In the model, RESECV of linalool and linalyl acetate were 0.170 and 0.416, respectively; RM-SEP were 0.188 and 0.364. The results indicated that raw data was pretreated by OSC and FiPLS, the NIR-PLS quantitative analysis model with good robustness, high measurement precision; it could quickly determine the content of linalool and linalyl acetate in lavender essential oil. In addition, the model has a favorable prediction ability. The study also provide a new effective method which could rapid quantitative analysis the major components of Xinjiang lavender essential oil.

High-sensitivity determination of Zn(II) and Cu(II) in vitro by fluorescence polarization

NASA Astrophysics Data System (ADS)

Thompson, Richard B.; Maliwal, Badri P.; Feliccia, Vincent; Fierke, Carol A.

1998-04-01

Recent work has suggested that free Cu(II) may play a role in syndromes such as Crohn's and Wilson's diseases, as well as being a pollutant toxic at low levels to shellfish and sheep. Similarly, Zn(II) has been implicated in some neural damage in the brain resulting from epilepsy and ischemia. Several high sensitivity methods exist for determining these ions in solution, including GFAAS, ICP-MS, ICP-ES, and electrochemical techniques. However, these techniques are generally slow and costly, require pretreatment of the sample, require complex instruments and skilled personnel, and are incapable of imaging at the cellular and subcellular level. To address these shortcomings we developed fluorescence polarization (anisotropy) biosensing methods for these ions which are very sensitivity, highly selective, require simple instrumentation and little pretreatment, and are inexpensive. Thus free Cu(II) or Zn(II) can be determined at picomolar levels by changes in fluorescence polarization, lifetime, or wavelength ratio using these methods; these techniques may be adapted to microscopy.

Pretreatment of rapeseed straw by sodium hydroxide.

PubMed

Kang, Kyeong Eop; Jeong, Gwi-Taek; Park, Don-Hee

2012-06-01

Pretreatment method for rapeseed straw by sodium hydroxide was investigated for production of bioethanol and biobutanol. Various pretreatment parameters, including temperature, time, and sodium hydroxide concentration were optimized using a statistical method which is a central composite design of response surface methodology. In the case of sodium hydroxide pretreatment, optimal pretreatment conditions were found to be 7.9% sodium hydroxide concentration, 5.5 h of reaction time, and 68.4 °C of reaction temperature. The maximum glucose yield which can be recovered by enzymatic hydrolysis at the optimum conditions was 95.7% and the experimental result was 94.0 ± 4.8%. This experimental result was in agreement with the model prediction. An increase of surface area and pore size in pretreated rapeseed straw by sodium hydroxide pretreatment was observed by scanning electron microscope.

Pretreatment Solution for Water Recovery Systems

NASA Technical Reports Server (NTRS)

Muirhead, Dean (Inventor)

2018-01-01

Chemical pretreatments are used to produce usable water by treating a water source with a chemical pretreatment that contains a hexavalent chromium and an acid to generate a treated water source, wherein the concentration of sulfate compounds in the acid is negligible, and wherein the treated water source remains substantially free of precipitates after the addition of the chemical pretreatment. Other methods include reducing the pH in urine to be distilled for potable water extraction by pretreating the urine before distillation with a pretreatment solution comprising one or more acid sources selected from a group consisting of phosphoric acid, hydrochloric acid, and nitric acid, wherein the urine remains substantially precipitate free after the addition of the pretreatment solution. Another method described comprises a process for reducing precipitation in urine to be processed for water extraction by mixing the urine with a pretreatment solution comprising hexavalent chromium compound and phosphoric acid.

Levosimendan: A Cardiovascular Drug to Prevent Liver Ischemia-Reperfusion Injury?

PubMed Central

Fulop, Andras; Rosero, Oliver; Garbaisz, David; Turoczi, Zsolt; Lotz, Gabor; Rakonczay, Zoltan; Balla, Zsolt; Hegedus, Viktor; Harsanyi, Laszlo; Szijarto, Attila

2013-01-01

Introduction Temporary occlusion of the hepatoduodenal ligament leads to an ischemic-reperfusion (IR) injury in the liver. Levosimendan is a new positive inotropic drug, which induces preconditioning-like adaptive mechanisms due to opening of mitochondrial KATP channels. The aim of this study was to examine possible protective effects of levosimendan in a rat model of hepatic IR injury. Material and Methods Levosimendan was administered to male Wistar rats 1 hour (early pretreatment) or 24 hours (late pretreatment) before induction of 60-minute segmental liver ischemia. Microcirculation of the liver was monitored by laser Doppler flowmeter. After 24 hours of reperfusion, liver and blood samples were taken for histology, immuno- and enzyme-histochemistry (TUNEL; PARP; NADH-TR) as well as for laboratory tests. Furthermore, liver antioxidant status was assessed and HSP72 expression was measured. Results In both groups pretreated with levosimendan, significantly better hepatic microcirculation was observed compared to respective IR control groups. Similarly, histological damage was also reduced after levosimendan administration. This observation was supported by significantly lower activities of serum ALT (pearly = 0.02; plate = 0.005), AST (pearly = 0.02; plate = 0.004) and less DNA damage by TUNEL test (pearly = 0.05; plate = 0.034) and PAR positivity (pearly = 0.02; plate = 0.04). Levosimendan pretreatment resulted in significant improvement of liver redox homeostasis. Further, significantly better mitochondrial function was detected in animals receiving late pretreatment. Finally, HSP72 expression was increased by IR injury, but it was not affected by levosimendan pretreatment. Conclusion Levosimendan pretreatment can be hepatoprotective and it could be useful before extensive liver resection. PMID:24040056

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Simultaneous determination of 15 marker constituents in various radix Astragali preparations by solid-phase extraction and high-performance liquid chromatography.

PubMed

Qi, Lian-Wen; Yu, Qing-Tao; Yi, Ling; Ren, Mei-Ting; Wen, Xiao-Dong; Wang, Yu-Xia; Li, Ping

2008-01-01

An improved quality control method was developed to simultaneously determine 15 major constituents (eight flavonoids and seven saponins) in various radix Astragali preparations, using SPE for pretreatment of samples, HPLC with diode-array and evaporative light scattering detectors (DAD-ELSD) for quantification in one run, and HPLC-ESI-TOF/MS for definite identification of compounds in preparations. Optimum separations were obtained with a ZORBAX C(18) column, using a gradient elution with 0.3% aqueous formic acid and ACN. This established method was fully validated with respect to linearity, precision, repeatability, and accuracy, and was successfully applied to quantify the 15 compounds in 19 commercial samples, including 3 dosage forms, i. e., oral solution, injection, concentrated granule, and its processed products of radix Astragali. The results demonstrated that many factors might result in significant differences in quality of the final preparations, including crude drugs, pretreatment processes, manufacturing procedure, storage conditions, etc. Then the developed method provided a reasonable and powerful manner to ensure the efficacy, safety, and batch-to-batch uniformity of radix Astragali products by standardizing each procedure, and thus should be proposed as quality control for the clinical use and modernization of herbal preparations.

Irradiation dose detection of irradiated milk powder using visible and near-infrared spectroscopy and chemometrics.

PubMed

Kong, W W; Zhang, C; Liu, F; Gong, A P; He, Y

2013-08-01

The objective of this study was to examine the possibility of applying visible and near-infrared spectroscopy to the quantitative detection of irradiation dose of irradiated milk powder. A total of 150 samples were used: 100 for the calibration set and 50 for the validation set. The samples were irradiated at 5 different dose levels in the dose range 0 to 6.0 kGy. Six different pretreatment methods were compared. The prediction results of full spectra given by linear and nonlinear calibration methods suggested that Savitzky-Golay smoothing and first derivative were suitable pretreatment methods in this study. Regression coefficient analysis was applied to select effective wavelengths (EW). Less than 10 EW were selected and they were useful for portable detection instrument or sensor development. Partial least squares, extreme learning machine, and least squares support vector machine were used. The best prediction performance was achieved by the EW-extreme learning machine model with first-derivative spectra, and correlation coefficients=0.97 and root mean square error of prediction=0.844. This study provided a new approach for the fast detection of irradiation dose of milk powder. The results could be helpful for quality detection and safety monitoring of milk powder. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Innovative UVC light (185 nm) and radio-frequency-plasma pretreatment of Nylon surfaces at atmospheric pressure and their implications in photocatalytic processes.

PubMed

Mejía, M I; Marín, J M; Restrepo, G; Pulgarín, C; Mielczarski, E; Mielczarski, J; Stolitchnov, I; Kiwi, J

2009-10-01

Innovative pretreatment by UVC light (185 nm) and by radio-frequency (RF) plasma at atmospheric pressure to functionalize the Nylon surface, increasing its bondability toward TiO(2), is reported in this study. In the case of UVC light pretreatment in air, the molar absorption coefficient of O(2)/N(2) at 185 nm is very low and the air in the chamber absorbs very little light from the UVC source before reaching the Nylon sample. Nylon fabrics under RF plasma were also functionalized at atmospheric pressure because of the marked heating effect introduced in the Nylon by the RF plasma. This effect leads to intermolecular bond breaking and oxygenated surface groups in the topmost Nylon layers. Both pretreatments enhanced significantly the photocatalytic discoloration of the red-wine stain in Nylon-TiO(2) compared with samples without pretreatment. The UVC and RF methods in the absence of vacuum imply a considerable cost reduction to functionalize textile surfaces, suggesting a potential industrial application. Red-wine-stain discoloration under simulated sunlight was monitored quantitatively by diffuse-reflectance spectroscopy and by CO(2) evolution. X-ray photoelectron spectroscopy (XPS) was used to monitor the changes of the C, N, and S species on the Nylon topmost layers during the discoloration process. Significant changes in the XPS spectra of Ti 2p peaks were observed during discoloration of the wine spots. Wine stains attenuated the signal of the Ti 2p (458.4 eV) peak in the Nylon-TiO(2)-stained wine sample at time zero (from now on, the time before the discoloration process). Furthermore, a decrease of the wine-related O 1s signal at 529.7 eV and N 1s signal at 399.5 eV was observed during the discoloration process, indicating an efficient catalytic decomposition of the wine pigment on Nylon-TiO(2). X-ray diffraction detected the formation of anatase on the Nylon fibers. High-resolution transmission electron microscopy shows the formation of anatase particles with sizes between 8 and 20 nm.

Residual antibiofilm effects of various concentrations of double antibiotic paste used during regenerative endodontics after different application times.

PubMed

Jenks, Daniel B; Ehrlich, Ygal; Spolnik, Kenneth; Gregory, Richard L; Yassen, Ghaeth H

2016-10-01

We investigated the residual antibiofilm effects of different concentrations of double antibiotic paste (DAP) applied on radicular dentin for 1 or 4 weeks. Dentin samples were prepared (n=120), sterilized and pretreated for 1 or 4 weeks with the clinically used concentration of DAP (500mg/mL), low concentrations of DAP (1, 5 or 50mg/mL) loaded into a methylcellulose system, calcium hydroxide (Ca(OH) 2 ), or placebo paste. After the assigned treatment time, treatment pastes were rinsed off and the samples were kept independently in phosphate buffered saline for 3 weeks. Pretreated dentin samples were then inoculated with Enterococcus faecalis and bacterial biofilms were allowed to grow for an additional 3 weeks. Biofilms were then retrieved from dentin using biofilm disruption assays, diluted, spiral plated, and quantified. Fisher's Exact and Wilcoxon rank sum tests were used for statistical comparisons (α=0.05). Dentin pretreatment for 4 weeks with 5, 50 or 500mg/mL of DAP demonstrated significantly higher residual antibiofilm effects and complete eradication of E. faecalis biofilms in comparison to a 1 week pretreatment with similar concentrations. However, dentin pretreated with 1mg/mL of DAP or Ca(OH) 2 did not provide a substantial residual antibiofilm effect regardless of the application time. Dentin pretreatment with 5mg/mL of DAP or higher for 4 weeks induced significantly higher residual antibiofilm effects in comparison to a 1 week pretreatment with the same concentrations. Copyright © 2016 Elsevier Ltd. All rights reserved.

Method to separate lignin-rich solid phase from acidic biomass suspension at an acidic pH

DOEpatents

Yasarla, Kumar Lakshmi Rakesh; Ramarao, Bandaru V; Amidon, Thomas

2017-09-05

A method of separating a lignin-rich solid phase from a solution suspension, by pretreating a lignocellulosic biomass with a pretreatment fluid having remove soluble components, colloidal material and primarily lignin containing particles; separating the pretreated lignocellulosic biomass from the pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles; flocculating the separated pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles using polyethylene oxide (i.e., PEO) or cationic Poly acrylamide (i.e., CPAM) as a flocculating agent; and filtering the flocculated separated pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles to remove agglomerates.

Long-term bonding effectiveness of simplified etch-and-rinse adhesives to dentin after different surface pre-treatments

PubMed Central

Verma, Radhika; Singh, Udai Pratap; Tyagi, Shashi Prabha; Nagpal, Rajni; Manuja, Naveen

2013-01-01

Objective: To evaluate the effect of 2% chlorhexidine (CHX) and 30% proanthocyanidin (PA) application on the immediate and long-term bond strength of simplified etch-and-rinse adhesives to dentin. Materials and Methods: One hundred twenty extracted human molar teeth were ground to expose the flat dentin surface. The teeth were equally divided into six groups according to the adhesives used, either Tetric N Bond or Solobond M and pretreatments given either none, CHX, or PA. Composite cylinder was bonded to each specimen using the respective adhesive technique. Half the samples from each group (n = 10) were then tested immediately. The remaining samples were tested after 6 month storage in distilled water. Results: The mean bond strength of samples was not significantly different upon immediate testing being in the range of 8.4(±0.7) MPa. The bond strength fell dramatically in the control specimens after 6 month storage to around 4.7(±0.33) MPa, while the bond strength was maintained in the samples treated with both CHX and PA. Conclusion: Thirty percent PA was comparable to 2% CHX with respect to preservation of the resin dentin bond over 6 months. PMID:23956543

How chip size impacts steam pretreatment effectiveness for biological conversion of poplar wood into fermentable sugars

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeMartini, Jaclyn D.; Foston, Marcus; Meng, Xianzhi

We report that woody biomass is highly recalcitrant to enzymatic sugar release and often requires significant size reduction and severe pretreatments to achieve economically viable sugar yields in biological production of sustainable fuels and chemicals. However, because mechanical size reduction of woody biomass can consume significant amounts of energy, it is desirable to minimize size reduction and instead pretreat larger wood chips prior to biological conversion. To date, however, most laboratory research has been performed on materials that are significantly smaller than applicable in a commercial setting. As a result, there is a limited understanding of the effects that largermore » biomass particle size has on the effectiveness of steam explosion pretreatment and subsequent enzymatic hydrolysis of wood chips. To address these concerns, novel downscaled analysis and high throughput pretreatment and hydrolysis (HTPH) were applied to examine whether differences exist in the composition and digestibility within a single pretreated wood chip due to heterogeneous pretreatment across its thickness. Heat transfer modeling, Simons’ stain testing, magnetic resonance imaging (MRI), and scanning electron microscopy (SEM) were applied to probe the effects of pretreatment within and between pretreated wood samples to shed light on potential causes of variation, pointing to enzyme accessibility (i.e., pore size) distribution being a key factor dictating enzyme digestibility in these samples. Application of these techniques demonstrated that the effectiveness of pretreatment of Populus tremuloides can vary substantially over the chip thickness at short pretreatment times, resulting in spatial digestibility effects and overall lower sugar yields in subsequent enzymatic hydrolysis. Finally, these results indicate that rapid decompression pretreatments (e.g., steam explosion) that specifically alter accessibility at lower temperature conditions are well suited for larger wood chips due to the non-uniformity in temperature and digestibility profiles that can result from high temperature and short pretreatment times. Furthermore, this study also demonstrated that wood chips were hydrated primarily through the natural pore structure during pretreatment, suggesting that preserving the natural grain and transport systems in wood during storage and chipping processes could likely promote pretreatment efficacy and uniformity.« less

How chip size impacts steam pretreatment effectiveness for biological conversion of poplar wood into fermentable sugars

DOE PAGES

DeMartini, Jaclyn D.; Foston, Marcus; Meng, Xianzhi; ...

2015-12-09

We report that woody biomass is highly recalcitrant to enzymatic sugar release and often requires significant size reduction and severe pretreatments to achieve economically viable sugar yields in biological production of sustainable fuels and chemicals. However, because mechanical size reduction of woody biomass can consume significant amounts of energy, it is desirable to minimize size reduction and instead pretreat larger wood chips prior to biological conversion. To date, however, most laboratory research has been performed on materials that are significantly smaller than applicable in a commercial setting. As a result, there is a limited understanding of the effects that largermore » biomass particle size has on the effectiveness of steam explosion pretreatment and subsequent enzymatic hydrolysis of wood chips. To address these concerns, novel downscaled analysis and high throughput pretreatment and hydrolysis (HTPH) were applied to examine whether differences exist in the composition and digestibility within a single pretreated wood chip due to heterogeneous pretreatment across its thickness. Heat transfer modeling, Simons’ stain testing, magnetic resonance imaging (MRI), and scanning electron microscopy (SEM) were applied to probe the effects of pretreatment within and between pretreated wood samples to shed light on potential causes of variation, pointing to enzyme accessibility (i.e., pore size) distribution being a key factor dictating enzyme digestibility in these samples. Application of these techniques demonstrated that the effectiveness of pretreatment of Populus tremuloides can vary substantially over the chip thickness at short pretreatment times, resulting in spatial digestibility effects and overall lower sugar yields in subsequent enzymatic hydrolysis. Finally, these results indicate that rapid decompression pretreatments (e.g., steam explosion) that specifically alter accessibility at lower temperature conditions are well suited for larger wood chips due to the non-uniformity in temperature and digestibility profiles that can result from high temperature and short pretreatment times. Furthermore, this study also demonstrated that wood chips were hydrated primarily through the natural pore structure during pretreatment, suggesting that preserving the natural grain and transport systems in wood during storage and chipping processes could likely promote pretreatment efficacy and uniformity.« less

Highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite and nafion composite modified screen printed carbon electrode.

PubMed

Ku, Shuhao; Palanisamy, Selvakumar; Chen, Shen-Ming

2013-12-01

Herein, we report a highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite/nafion composite modified screen printed carbon (SPC) electrode. Electrochemically activated graphite/nafion composite was prepared by using a simple electrochemical method. Scanning electron microscope (SEM) used to characterize the surface morphology of the fabricated composite electrode. The SEM result clearly indicates that the graphitic basal planes were totally disturbed and leads to the formation of graphite nanosheets. The composite modified electrode showed an enhanced electrocatalytic activity toward the oxidation of DA when compared with either electrochemical pretreated graphite or nafion SPC electrodes. The fabricated composite electrode exhibits a good electrocatalytic oxidation toward DA in the linear response range from 0.5 to 70 μM with the detection limit of 0.023 μM. The proposed sensor also exhibits very good selectivity and stability, with the appreciable sensitivity. In addition, the proposed sensor showed satisfactory recovery results toward the commercial pharmaceutical DA samples. Copyright © 2013 Elsevier Inc. All rights reserved.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

PubMed Central

Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detection limits (LODs) in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples. PMID:29348966

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection.

PubMed

Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100  μ g/L for urine, 5-100  μ g/L for saliva, and 3-100  μ g/L for sweat samples with determination coefficients ( R ) > 0.992. Low detection limits (LODs) in the range of 1.8  μ g/L, 5.1  μ g/L, and 5.8  μ g/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

Perspective and prospective of pretreatment of corn straw for butanol production.

PubMed

Baral, Nawa Raj; Li, Jiangzheng; Jha, Ajay Kumar

2014-01-01

Corn straw, lignocellulosic biomass, is a potential substrate for microbial production of bio-butanol. Bio-butanol is a superior second generation biofuel among its kinds. Present researches are focused on the selection of butanol tolerant clostridium strain(s) to optimize butanol yield in the fermentation broth because of toxicity of bio-butanol to the clostridium strain(s) itself. However, whatever the type of the strain(s) used, pretreatment process always affects not only the total sugar yield before fermentation but also the performance and growth of microbes during fermentation due to the formation of hydroxyl-methyl furfural, furfural and phenolic compounds. In addition, the lignocellulosic biomasses also resist physical and biological attacks. Thus, selection of best pretreatment process and its parameters is crucial. In this context, worldwide research efforts are increased in past 12 years and researchers are tried to identify the best pretreatment method, pretreatment conditions for the actual biomass. In this review, effect of particle size, status of most common pretreatment method and enzymatic hydrolysis particularly for corn straw as a substrate is presented. This paper also highlights crucial parameters necessary to consider during most common pretreatment processes such as hydrothermal, steam explosion, ammonia explosion, sulfuric acid, and sodium hydroxide pretreatment. Moreover, the prospective of pretreatment methods and challenges is discussed.

Fundamental characteristics of microwave explosion pretreatment of wood. I, Properties of temperature development

Treesearch

Xian-jun Li; Ke-yang Lu; Lan-ying Lin; Yong-dong Zhou; Zhi-yong Cai; Feng Fu

2010-01-01

In this study, the effects of microwave radiation intensity, radiation time and initial wood moisture content (MC) on the properties of temperature development in Eucalyptus urophylla wood samples during the microwave explosion pretreatment have been investigated using a new microwave pretreatment equipment. The results show that 1) with the increase of microwave...

A rapid and simple pretreatment method for benzoylurea insecticides in honey samples using in-syringe dispersive liquid-liquid microextraction based on the direct solidification of ionic liquids.

PubMed

Wang, Huazi; Hu, Lu; Li, Wanzhen; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

2016-11-04

A pretreatment method using in-syringe dispersive liquid-liquid microextraction based on the direct solidification of ionic liquids before high performance liquid chromatography analysis was developed for the determination of benzoylurea insecticides (BUs) in honey samples. The hydrophobic ionic liquid [N 4444 ][PF 6 ], formed in situ by the hydrophilic ionic liquid [N 4444 ]Cl and the ion exchange reagent KPF 6 , was used to extract the target analytes. The entire extraction procedure was performed in a syringe. The extractant was solidified at room temperature and collected using a nylon membrane filter. This technique did not require a dispersive solvent, vortex mixer, ultrasound bath, or centrifugation. The parameters affecting the extraction efficiency were investigated through an experimental design. Under the optimal conditions, the limits of detection for the four BUs varied from 0.21 to 0.42μgL -1 in solution (2.1-4.2μgkg -1 in honey). Good linearities were obtained in the range of 2-300μgL -1 , with coefficients of determination greater than 0.999. The recoveries of the four BUs ranged from 80.94% to 84.59%. The intra-day (n=3) and inter-day (n=3) relative standard deviations were less than 5.08%. Finally, the proposed method was applied to the determination of BUs in commercial honey samples with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

Conditioning of renewable silver amalgam film electrode for the characterization of clothianidin and its determination in selected samples by adsorptive square-wave voltammetry.

PubMed

Brycht, Mariola; Skrzypek, Sławomira; Guzsvány, Valéria; Berenji, Janoš

2013-12-15

A new square-wave adsorptive stripping voltammetric (SWAdSV) method was developed for the determination of the neonicotinoid insecticide clothianidin (Clo), based on its reduction at a renewable silver amalgam film electrode (Hg(Ag)FE). The key point of the procedure is the pretreatment of the Hg(Ag)FE by applying the appropriate conditioning potential (-1.70 V vs. Ag/AgCl reference electrode). Under the optimized voltammetric conditions, such pretreatment resulted in the peak for the Clo reduction in Britton-Robinson buffer pH 9.0 at about -0.60 V, which was used for the analytical purpose. The developed SWAdSV procedure made it possible to determine Clo in the concentration range of 6.0×10(-7)-7.0×10(-6) mol L(-1) (LOD=1.8×10(-7) mol L(-1), LOQ=6.0×10(-7) mol L(-1)) and 7.0×10(-6)-4.0×10(-5) mol L(-1) (LOD=1.3×10(-6) mol L(-1), LOQ=4.2×10(-6) mol L(-1)). The repeatability, precision, and the recovery of the method were determined. The effect of common interfering pesticides was also investigated. Standard addition method was successfully applied and validated for the determination of Clo in spiked Warta River water, corn seeds samples, and in corn seeds samples treated with the commercial formulation PONCHO 600 FS. © 2013 Elsevier B.V. All rights reserved.

Gravimetric screening method for fungal decay of paper: inoculation with Trametes versicolor.

PubMed

Råberg, Ulrika; Hafrén, Jonas

2009-10-01

The European standard test EN 113 for fungal degradation of solid wood has been adapted for degradation of paper by white rot fungus (Trametes versicolor). Fungal degradation of paper sheets may potentially be used for screening different wood preservatives on paper instead of solid wood. The paper samples showed higher relative mass losses compared to wood, and samples pretreated with boric acid, copper sulfate and polymerized linseed oil were successfully tested for biodegradation using the paper sheet method. The results on paper degradation were compared with wood, both as wood blocks (according to standard test) and wood cut in sections forming layered structures mimicking paper layers.

Stable isotope dilution analysis of hydrologic samples by inductively coupled plasma mass spectrometry

USGS Publications Warehouse

Garbarino, John R.; Taylor, Howard E.

1987-01-01

Inductively coupled plasma mass spectrometry is employed in the determination of Ni, Cu, Sr, Cd, Ba, Ti, and Pb in nonsaline, natural water samples by stable isotope dilution analysis. Hydrologic samples were directly analyzed without any unusual pretreatment. Interference effects related to overlapping isobars, formation of metal oxide and multiply charged ions, and matrix composition were identified and suitable methods of correction evaluated. A comparability study snowed that single-element isotope dilution analysis was only marginally better than sequential multielement isotope dilution analysis. Accuracy and precision of the single-element method were determined on the basis of results obtained for standard reference materials. The instrumental technique was shown to be ideally suited for programs associated with certification of standard reference materials.

Improvement of enzymatic hydrolysis and ethanol production from corn stalk by alkali and N-methylmorpholine-N-oxide pretreatments.

PubMed

Cai, Ling-Yan; Ma, Yu-Long; Ma, Xiao-Xia; Lv, Jun-Min

2016-07-01

A combinative technology of alkali and N-methylmorpholine-N-oxide (NMMO) was used to pretreat corn stalk (CS) for improving the efficiencies of subsequent enzymatic hydrolysis and ethanol fermentation. The results showed that this strategy could not only remove hemicellulose and lignin but also decrease the crystallinity of cellulose. About 98.0% of enzymatic hydrolysis yield was obtained from the pretreated CS as compared with 46.9% from the untreated sample. The yield for corresponding ethanol yield was 64.6% while untreated CS was only 18.8%. Besides, xylose yield obtained from the untreated CS was only 11.1%, while this value was 93.8% for alkali with NMMO pretreated sample. These results suggest that a combination of alkali with 50% (wt/wt) NMMO solution may be a promising alternative for pretreatment of lignocellulose, which can increase the productions of subsequent enzymatic hydrolysis and ethanol fermentation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Understanding changes in cellulose crystalline structure of lignocellulosic biomass during ionic liquid pretreatment by XRD.

PubMed

Zhang, Jiafu; Wang, Yixun; Zhang, Liye; Zhang, Ruihong; Liu, Guangqing; Cheng, Gang

2014-01-01

X-ray diffraction (XRD) was used to understand the interactions of cellulose in lignocellulosic biomass with ionic liquids (ILs). The experiment was designed in such a way that the process of swelling and solubilization of crystalline cellulose in plant cell walls was followed by XRD. Three different feedstocks, switchgrass, corn stover and rice husk, were pretreated using 1-butyl-3-methylimidazolium acetate ([C4mim][OAc]) at temperatures of 50-130°C for 6h. At a 5 wt.% biomass loading, increasing pretreatment temperature led to a drop in biomass crystallinity index (CrI), which was due to swelling of crystalline cellulose. After most of the crystalline cellulose was swollen with IL molecules, a low-order structure was found in the pretreated samples. Upon further increasing temperature, cellulose II structure started to form in the pretreated biomass samples as a result of solubilization of cellulose in [C4mim][OAc] and subsequent regeneration. Copyright © 2013 Elsevier Ltd. All rights reserved.

Evaluation energy efficiency of bioconversion knot rejects to ethanol in comparison to other thermochemically pretreated biomass.

PubMed

Wang, Zhaojiang; Qin, Menghua; Zhu, J Y; Tian, Guoyu; Li, Zongquan

2013-02-01

Rejects from sulfite pulp mill that otherwise would be disposed of by incineration were converted to ethanol by a combined physical-biological process that was comprised of physical refining and simultaneous saccharification and fermentation (SSF). The energy efficiency was evaluated with comparison to thermochemically pretreated biomass, such as those pretreated by dilute acid (DA) and sulfite pretreatment to overcome recalcitrance of lignocelluloses (SPORL). It was observed that the structure deconstruction of rejects by physical refining was indispensable to effective bioconversion but more energy intensive than that of thermochemically pretreated biomass. Fortunately, the energy consumption was compensated by the reduced enzyme dosage and the elevated ethanol yield. Furthermore, adjustment of disk-plates gap led to reduction in energy consumption with negligible influence on ethanol yield. In this context, energy efficiency up to 717.7% was achieved for rejects, much higher than that of SPORL sample (283.7%) and DA sample (152.8%). Copyright © 2012 Elsevier Ltd. All rights reserved.

Understanding Treatment Readiness in Recently Assessed, Pre-Treatment Substance Abusers

PubMed Central

Rapp, Richard C.; Xu, Jiangmin; Carr, Carey A.; Timothy Lane, D.; Redko, Cristina; Wang, Jichuan; Carlson, Robert G.

2007-01-01

The goal of this study was to more fully understand readiness for treatment in a pre-treatment sample of 446 substance abusers. Structural Equation Modeling (SEM) was used to: (1) examine the relationships between readiness factors identified in the Pre-Treatment Readiness Scale; and (2) identify the effects of predisposing, illness, and inhibiting determinants on the factors. As with in-treatment samples, Problem Recognition was found to influence Treatment Readiness, although through a different intervening factor, Desire for Change rather than Desire for Help. A fourth factor, Treatment Reluctance, was also influenced by the Desire for Change factor. Fixed characteristics such as age and gender had minimal influences on readiness factors, as did inhibiting characteristics that reflected recent functioning. Illness characteristics including drug severity and perceived treatment barriers had a more robust influence on readiness factors. This study provides an increased understanding of readiness for treatment among pre-treatment substance abusers and also supported the construct validity of the Pre-Treatment Readiness Scale. PMID:19274847

Synthesis of cross-linked chitosan modified with the glycine moiety for the collection/concentration of bismuth in aquatic samples for ICP-MS determination.

PubMed

Oshita, Koji; Noguchi, Osamu; Oshima, Mitsuko; Motomizu, Shoji

2007-10-01

A chelating resin, cross-linked chitosan modified with the glycine moiety (glycine-type chitosan resin), was developed for the collection and concentration of bismuth in aquatic samples for ICP-MS measurements. The adsorption behavior of bismuth and 55 elements on glycine-type chitosan resin was systematically examined by passing a sample solution containing 56 elements through a mini-column packed with the resin (wet volume; 1 ml). After eluting the elements adsorbed on the resin with nitric acid, the eluates were measured by ICP-MS. The glycine-type chitosan resin could adsorb several cations by a chelating mechanism and several oxoanions by an anion-exchange mechanism. Especially, the resin could adsorb almost 100% Bi(III) over a wide pH region from pH 2 to 6. Bismuth could be strongly adsorbed at pH 3, and eluted quantitatively with 10 ml of 3 M nitric acid. A column pretreatment method with the glycine-type chitosan resin was used prior to removal of high concentrations of matrices in a seawater sample and the preconcentration of trace bismuth in river water samples for ICP-MS measurements. The column pretreatment method was also applied to the determination of bismuth in real samples by ICP-MS. The LOD of bismuth was 0.1 pg ml(-1) by 10-fold column preconcentration for ICP-MS measurements. The analytical results for bismuth in sea and river water samples by ICP-MS were 22.9 +/- 0.5 pg ml(-1) (RSD, 2.2%) and 2.08 +/- 0.05 pg ml(-1) (RSD, 2.4%), respectively.

Strategies for characterizing compositions of industrial pulp and paper sludge

NASA Astrophysics Data System (ADS)

Aslanzadeh, Solmaz; Kemal, Rahmat A.; Pribowo, Amadeus Y.

2018-01-01

The large quantities of waste sludge produced by the pulp and paper industry present significant environmental challenges. In order to minimize the amounts of waste, the pulp sludge should be utilized for productive applications. In order to find feasible solutions, the sludge need to be characterized. In this study, the potential of using acid pretreatment and ashing method to determine the chemical compositions of the sludge is investigated. This study shows that acid pretreatment could be used to dissolve and determine the composition of CaCO3 in the pulp sludge. CaCO3 removal also facilitates the measurement of fiber and ash (clay) contents by using the ashing method. The optimum acid concentration used to completely dissolve CaCO3 was determined using a titration method. Using this method, the measurement of the chemical composition of the sludge sample revealed that it consisted primarily of CaCO3 (55% w/w), clay (25%, w/w), and fibers (18%, w/w). Based on these chemical compositions, potential utilization for the sludge could be determined.

Fast pyrolysis of tropical biomass species and influence of water pretreatment on product distributions

DOE PAGES

Morgan, Trevor James; Turn, Scott Q.; Sun, Ning; ...

2016-03-15

Here, the fast pyrolysis behaviour of pretreated banagrass was examined at four temperatures (between 400 and 600 C) and four residence times (between ~1.2 and 12 s). The pretreatment used water washing/leaching to reduce the inorganic content of the banagrass. Yields of bio-oil, permanent gases and char were determined at each reaction condition and compared to previously published results from untreated banagrass. Comparing the bio-oil yields from the untreated and pretreated banagrass shows that the yields were greater from the pretreated banagrass by 4 to 11 wt% (absolute) at all reaction conditions. The effect of pretreatment (i.e. reducing the amountmore » of ash, and alkali and alkali earth metals) on pyrolysis products is: 1) to increase the dry bio-oil yield, 2) to decrease the amount of undetected material, 3) to produce a slight increase in CO yield or no change, 4) to slightly decrease CO 2 yield or no change, and 5) to produce a more stable bio-oil (less aging). Char yield and total gas yield were unaffected by feedstock pretreatment. Four other tropical biomass species were also pyrolyzed under one condition (450°C and 1.4 s residence time) for comparison to the banagrass results. The samples include two hardwoods: leucaena and eucalyptus, and two grasses: sugarcane bagasse and energy-cane. A sample of pretreated energy-cane was also pyrolyzed. Of the materials tested, the best feedstocks for fast pyrolysis were sugarcane bagasse, pretreated energy cane and eucalyptus based on the yields of 'dry bio-oil', CO and CO 2. On the same basis, the least productive feedstocks are untreated banagrass followed by pretreated banagrass and leucaena.« less

Fast pyrolysis of tropical biomass species and influence of water pretreatment on product distributions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morgan, Trevor James; Turn, Scott Q.; Sun, Ning

Here, the fast pyrolysis behaviour of pretreated banagrass was examined at four temperatures (between 400 and 600 C) and four residence times (between ~1.2 and 12 s). The pretreatment used water washing/leaching to reduce the inorganic content of the banagrass. Yields of bio-oil, permanent gases and char were determined at each reaction condition and compared to previously published results from untreated banagrass. Comparing the bio-oil yields from the untreated and pretreated banagrass shows that the yields were greater from the pretreated banagrass by 4 to 11 wt% (absolute) at all reaction conditions. The effect of pretreatment (i.e. reducing the amountmore » of ash, and alkali and alkali earth metals) on pyrolysis products is: 1) to increase the dry bio-oil yield, 2) to decrease the amount of undetected material, 3) to produce a slight increase in CO yield or no change, 4) to slightly decrease CO 2 yield or no change, and 5) to produce a more stable bio-oil (less aging). Char yield and total gas yield were unaffected by feedstock pretreatment. Four other tropical biomass species were also pyrolyzed under one condition (450°C and 1.4 s residence time) for comparison to the banagrass results. The samples include two hardwoods: leucaena and eucalyptus, and two grasses: sugarcane bagasse and energy-cane. A sample of pretreated energy-cane was also pyrolyzed. Of the materials tested, the best feedstocks for fast pyrolysis were sugarcane bagasse, pretreated energy cane and eucalyptus based on the yields of 'dry bio-oil', CO and CO 2. On the same basis, the least productive feedstocks are untreated banagrass followed by pretreated banagrass and leucaena.« less

Fast Pyrolysis of Tropical Biomass Species and Influence of Water Pretreatment on Product Distributions

PubMed Central

Morgan, Trevor James; Turn, Scott Q.; Sun, Ning; George, Anthe

2016-01-01

The fast pyrolysis behaviour of pretreated banagrass was examined at four temperatures (between 400 and 600 C) and four residence times (between ~1.2 and 12 s). The pretreatment used water washing/leaching to reduce the inorganic content of the banagrass. Yields of bio-oil, permanent gases and char were determined at each reaction condition and compared to previously published results from untreated banagrass. Comparing the bio-oil yields from the untreated and pretreated banagrass shows that the yields were greater from the pretreated banagrass by 4 to 11 wt% (absolute) at all reaction conditions. The effect of pretreatment (i.e. reducing the amount of ash, and alkali and alkali earth metals) on pyrolysis products is: 1) to increase the dry bio-oil yield, 2) to decrease the amount of undetected material, 3) to produce a slight increase in CO yield or no change, 4) to slightly decrease CO2 yield or no change, and 5) to produce a more stable bio-oil (less aging). Char yield and total gas yield were unaffected by feedstock pretreatment. Four other tropical biomass species were also pyrolyzed under one condition (450°C and 1.4 s residence time) for comparison to the banagrass results. The samples include two hardwoods: leucaena and eucalyptus, and two grasses: sugarcane bagasse and energy-cane. A sample of pretreated energy-cane was also pyrolyzed. Of the materials tested, the best feedstocks for fast pyrolysis were sugarcane bagasse, pretreated energy cane and eucalyptus based on the yields of 'dry bio-oil', CO and CO2. On the same basis, the least productive feedstocks are untreated banagrass followed by pretreated banagrass and leucaena. PMID:26978265

Fast Pyrolysis of Tropical Biomass Species and Influence of Water Pretreatment on Product Distributions.

PubMed

Morgan, Trevor James; Turn, Scott Q; Sun, Ning; George, Anthe

2016-01-01

The fast pyrolysis behaviour of pretreated banagrass was examined at four temperatures (between 400 and 600 C) and four residence times (between ~1.2 and 12 s). The pretreatment used water washing/leaching to reduce the inorganic content of the banagrass. Yields of bio-oil, permanent gases and char were determined at each reaction condition and compared to previously published results from untreated banagrass. Comparing the bio-oil yields from the untreated and pretreated banagrass shows that the yields were greater from the pretreated banagrass by 4 to 11 wt% (absolute) at all reaction conditions. The effect of pretreatment (i.e. reducing the amount of ash, and alkali and alkali earth metals) on pyrolysis products is: 1) to increase the dry bio-oil yield, 2) to decrease the amount of undetected material, 3) to produce a slight increase in CO yield or no change, 4) to slightly decrease CO2 yield or no change, and 5) to produce a more stable bio-oil (less aging). Char yield and total gas yield were unaffected by feedstock pretreatment. Four other tropical biomass species were also pyrolyzed under one condition (450°C and 1.4 s residence time) for comparison to the banagrass results. The samples include two hardwoods: leucaena and eucalyptus, and two grasses: sugarcane bagasse and energy-cane. A sample of pretreated energy-cane was also pyrolyzed. Of the materials tested, the best feedstocks for fast pyrolysis were sugarcane bagasse, pretreated energy cane and eucalyptus based on the yields of 'dry bio-oil', CO and CO2. On the same basis, the least productive feedstocks are untreated banagrass followed by pretreated banagrass and leucaena.

Pretreatment of different biological matrices for exogenous testosterone analysis: a review.

PubMed

Pizzato, Edna Carolina; Filonzi, Marcelo; Rosa, Hemerson Silva da; de Bairros, André Valle

2017-11-01

The presence of exogenous testosterone has been monitored mainly in the urine and blood. However, other biological matrices such as hair, nail, and saliva samples can be used successfully for in vivo measurement. Chromatographic analysis requires pretreatment to obtain free testosterone and its metabolites. Among the pretreatment procedures, digestion, hydrolysis and solvolysis steps are conducted to reach the analytical purpose. Digestion assay is indicated for hair and nail samples. First, it is recommended to perform the decontamination step. After that, alkaline solution (NaOH), organic solvents and other reagents can be added to the samples and incubated under determined conditions for the digestion step. Hydrolysis assay is recommended to urine and blood samples. Acid hydrolysis cleaves conjugated testosterone and its metabolites using HCl or H 2 SO 4 solution at appropriate time and temperature. However, there is formation of interferent compounds, degradation of dehydroepiandrosterone and decrease of peak resolution for epitestosterone. Enzymatic hydrolysis is an alternative technique able to promote free testosterone and its metabolites with low degradation. It is important to establish the best conditions according to the biological fluid and the amount of the sample. Sulfatase enzyme is recommended together with β-glucuronidase to cleave sulfoconjugate steroids. Solvolysis assay is similar to acid hydrolysis, but organic solvents are responsible to promote steroid deconjugation. Other approaches such as combination of different pretreatments, surface response or ultrasonic energy have been used to obtain the total of free steroids. So, the biological matrix defines the best procedure for pretreatment to achieve the analytical purpose, knowing its advantages and limitations.

Direct Electrospray Ionization Mass Spectrometric Profiling of Real-World Samples via a Solid Sampling Probe

NASA Astrophysics Data System (ADS)

Yu, Zhan; Chen, Lee Chuin; Mandal, Mridul Kanti; Yoshimura, Kentaro; Takeda, Sen; Hiraoka, Kenzo

2013-10-01

This study presents a novel direct analysis strategy for rapid mass spectrometric profiling of biochemicals in real-world samples via a direct sampling probe (DSP) without sample pretreatments. Chemical modification is applied to a disposable stainless steel acupuncture needle to enhance its surface area and hydrophilicity. After insertion into real-world samples, biofluid can be attached on the DSP surface. With the presence of a high DC voltage and solvent vapor condensing on the tip of the DSP, analyte can be dissolved and electrosprayed. The simplicity in design, versatility in application aspects, and other advantages such as low cost and disposability make this new method a competitive tool for direct analysis of real-world samples.

Use of an online extraction liquid chromatography quadrupole time-of-flight tandem mass spectrometry method for the characterization of polyphenols in Citrus paradisi cv. Changshanhuyu peel.

PubMed

Tong, Chaoying; Peng, Mijun; Tong, Runna; Ma, Ruyi; Guo, Keke; Shi, Shuyun

2018-01-19

Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction of Citrus paradisi cv. Changshanhuyu (Changshanhuyu) peel, OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of twenty-two secondary metabolites were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and nine of them were discovered in Changshanhuyu peel for the first time to our knowledge. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparative evaluation of tensile bond strength of a polyvinyl acetate-based resilient liner following various denture base surface pre-treatment methods and immersion in artificial salivary medium: An in vitro study.

PubMed

Philip, Jacob M; Ganapathy, Dhanraj M; Ariga, Padma

2012-07-01

This study was formulated to evaluate and estimate the influence of various denture base resin surface pre-treatments (chemical and mechanical and combinations) upon tensile bond strength between a poly vinyl acetate-based denture liner and a denture base resin. A universal testing machine was used for determining the bond strength of the liner to surface pre-treated acrylic resin blocks. The data was analyzed by one-way analysis of variance and the t-test (α =.05). This study infers that denture base surface pre-treatment can improve the adhesive tensile bond strength between the liner and denture base specimens. The results of this study infer that chemical, mechanical, and mechano-chemical pre-treatments will have different effects on the bond strength of the acrylic soft resilient liner to the denture base. Among the various methods of pre-treatment of denture base resins, it was inferred that the mechano-chemical pre-treatment method with air-borne particle abrasion followed by monomer application exhibited superior bond strength than other methods with the resilient liner. Hence, this method could be effectively used to improve bond strength between liner and denture base and thus could minimize delamination of liner from the denture base during function.

Inhibitive effects of anti-oxidative vitamins on mannitol-induced apoptosis of vascular endothelial cells.

PubMed

Pan, Kai-yu; Shen, Mei-ping; Ye, Zhi-hong; Dai, Xiao-na; Shang, Shi-qiang

2006-10-01

Study blood vessel injury and gene expression indicating vascular endothelial cell apoptosis induced by mannitol with and without administration of anti-oxidative vitamins. Healthy rabbits were randomly divided into four groups. Mannitol was injected into the vein of the rabbit ear in each animal. Pre-treatment prior to mannitol injection was performed with normal saline (group B), vitamin C (group C) and vitamin E (group D). Blood vessel injury was assessed under electron and light microscopy. In a second experiment, cell culture specimen of human umbilical vein endothelial cells were treated with mannitol. Pre-treatment was done with normal saline (sample B), vitamin C (sample C) and vitamin E (sample D). Total RNA was extracted with the original single step procedure, followed by hybridisation and analysis of gene expression. In the animal experiment, serious blood vessel injury was seen in group A and group B. Group D showed light injury only, and normal tissue without pathological changes was seen in group C. Of all 330 apoptosis-related genes analysed in human cell culture specimen, no significant difference was seen after pre-treatment with normal saline, compared with the gene chip without pre-treatment. On the gene chip pre-treated with vitamin C, 45 apoptosis genes were down-regulated and 34 anti-apoptosis genes were up-regulated. Pre-treatment with vitamin E resulted in the down-regulation of 3 apoptosis genes. Vitamin C can protect vascular endothelial cells from mannitol-induced injury.

Fatty acids characterization, oxidative perspectives and consumer acceptability of oil extracted from pre-treated chia (Salvia hispanica L.) seeds.

PubMed

Imran, Muhammad; Nadeem, Muhammad; Manzoor, Muhammad Faisal; Javed, Amna; Ali, Zafar; Akhtar, Muhammad Nadeem; Ali, Muhammad; Hussain, Yasir

2016-09-20

Chia (Salvia hispanica L.) seeds have been described as a good source of lipids, protein, dietary fiber, polyphenolic compounds and omega-3 polyunsaturated fatty acids. The consumption of chia seed oil helps to improve biological markers related to metabolic syndrome diseases. The oil yield and fatty acids composition of chia oil is affected by several factors such as pre-treatment method and size reduction practices. Therefore, the main mandate of present investigate was to study the effect of different seed pre-treatments on yield, fatty acids composition and sensory acceptability of chia oil at different storage intervals and conditions. Raw chia seeds were characterized for proximate composition. Raw chia seeds after milling were passed through sieves to obtain different particle size fractions (coarse, seed particle size ≥ 10 mm; medium, seed particle size ≥ 5 mm; fine, seed particle size ≤ 5 mm). Heat pre-treatment of chia seeds included the water boiling (100 C°, 5 min), microwave roasting (900 W, 2450 MHz, 2.5 min), oven drying (105 ± 5 °C, 1 h) and autoclaving (121 °C, 15 lbs, 15 min) process. Extracted oil from pre-treated chia seeds were stored in Tin cans at 25 ± 2 °C and 4 ± 1 °C for 60-days and examined for physical (color, melting point, refractive index), oxidative (iodine value, peroxide value, free fatty acids), fatty acids (palmitic, stearic, oleic, linoleic, α-linolenic) composition and sensory (appearance, flavor, overall acceptability) parameters, respectively. The proximal composition of chia seeds consisted of 6.16 ± 0.24 % moisture, 34.84 ± 0.62 % oil, 18.21 ± 0.45 % protein, 4.16 ± 0.37 % ash, 23.12 ± 0.29 % fiber, and 14.18 ± 0.23 % nitrogen contents. The oil yield as a result of seed pre-treatments was found in the range of 3.43 ± 0.22 % (water boiled samples) to 32.18 ± 0.34 % (autoclaved samples). The oil samples at day 0 indicated the maximum color (R and Y Lovibond scale) value for oven drying while at storage day 60 (25 ± 2 °C), the highest color value was found for autoclave pre-treatment. The slightly increasing trend of color values for all treatments was observed during the storage period. The lowest iodine value (182.83 ± 1.18 g/100 g at storage day 0 & 173.49 ± 1.21 g/100 g at storage day 60, 25 ± 2 °C) was calculated for autoclaved samples while the maximum iodine value (193.42 ± 1.14 g/100 g at storage day 0 & 190.36 ± 1.17 g/100 g at storage day 60, 25 ± 2 °C) was recorded for raw chia samples. The significant increasing trend for all treatments was observed in case of peroxide value and free fatty acids production during storage. Maximum decrease in linoleic (35 %) and α-linolenic (18 %) fatty acids was observed in autoclaved samples. The oil from pre-treated seed samples obtained decreasing scores for sensory parameters throughout the storage period at different conditions. As a result, chia seeds are an important source of lipids and essential fatty acids. The water boiling and high temperature processing of chia seeds provides instability to lipids during storage at room temperature. However, detailed investigation is required on the processing performance and storage stability of food products supplemented with pre-treated chia seeds and furthers their effect on biological system.

Elucidation of Factors Effecting Enzymatic Saccharification using Transgenic Hardwoods

NASA Astrophysics Data System (ADS)

Min, Douyong

Three groups of transgenic wood samples were used as starting materials to elucidate the recalcitrance of enzymatic saccharification with/without pretreatments. The first group of transgenic wood samples is low lignin P. trichocarpa. The second group is low xylan P. trichocarpa. The third one is 12 hybrid poplars which have different levels of S/V ratio and lignin content. Four pretreatments were carried out in this research including dilute sulfuric acid, green liquor, auto hydrolysis and ozone delignification. The behavior among pretreatments as a function of removal of lignin appears to be different. Lignin is the major factor of recalcitrance of the lignocellulosic material to ethanol conversion process. Xylan also plays key role in this process. In addition, the crude milled wood lignin was isolated from these three groups of transgenic samples. Lignin carbohydrate complexes was characterized by 1H-13C HMQC and 13C NMR. Thus the effect of LCCs on enzymatic saccharification was elucidated. High S/V ratio propels the lignin removal during pretreatments however; high S/V ratio retards the enzymatic saccharification on the lignocellulosic material without pretreatments. The level of LCCs linkages accounts for additional recalcitrance of the lignocellulosic material to ethanol conversion process. The amount of LCCs linkages is affected by xylan content, lignin content and S/V ratio.

Testing of Candidate Polymeric Materials for Compatibility with Pure Alternate Pretreat as Part of the Universal Waste Management System (UWMS)

NASA Technical Reports Server (NTRS)

Wingard, C. D.

2018-01-01

The Universal Waste Management System (UWMS) is an improved Waste Collection System for astronauts living and working in low Earth orbit spacecraft. Polymeric materials used in water recovery on International Space Station are regularly exposed to phosphoric acid-treated 'pretreated' urine. Polymeric materials used in UWMS are not only exposed to pretreated urine, but also to concentrated phosphoric acid with oxidizer before dilution known as 'pure pretreat.' Samples of five different polymeric materials immersed in pure pretreat for 1 year were tested for liquid compatibility by measuring changes in storage modulus with a dynamic mechanical analyzer.

Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

PubMed

Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

2014-10-01

A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave assisted alkaline pretreatment to enhance enzymatic saccharification of catalpa sawdust.

PubMed

Jin, Shuguang; Zhang, Guangming; Zhang, Panyue; Li, Fan; Wang, Siqi; Fan, Shiyang; Zhou, Shuqiong

2016-12-01

Catalpa sawdust, a promising biofuel production biomass, was pretreated by microwave-water, -NaOH, and -Ca(OH) 2 to enhance enzymatic digestibility. After 48h enzymatic hydrolysis, microwave-Ca(OH) 2 pretreated sample showed the highest reducing sugar yield. The content of hemicellulose and lignin in catalpa sawdust decreased after microwave-alkali pretreatment. SEM observation showed that the catalpa sawdust surface with microwave-Ca(OH) 2 pretreatment suffered the most serious erosion. Crystallinity index of catalpa sawdust increased after all three kinds of pretreatment. The optimum conditions of microwave-Ca(OH) 2 pretreatment were particle size of 40mesh, Ca(OH) 2 dosage of 2.25% (w/v), microwave power of 400W, pretreatment time of 6min, enzyme loading of 175FPU/g, and hydrolysis time of 96h, and the reducing sugar yield of microwave-Ca(OH) 2 pretreated catalpa sawdust reached 402.73mg/g, which increased by 682.15% compared with that of raw catalpa sawdust. The catalpa sawdust with microwave-Ca(OH) 2 pretreatment is promising for biofuel production with great potential. Copyright © 2016 Elsevier Ltd. All rights reserved.

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

PubMed

van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

2002-09-01

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

Biological pretreatment of corn stover with white-rot fungus for improved enzymatic hydrolysis

USDA-ARS?s Scientific Manuscript database

Biological pretreatment of lignocellulosic biomass by white-rot fungus can represent a low-cost and eco-friendly alternative to harsh physical, chemical or physico-chemical pretreatment methods to facilitate enzymatic hydrolysis. However, fungal pretreatment can cause carbohydrate loss and it is, th...

Assessment of different pretreatment technologies for efficient bioconversion of lignocellulose to ethanol.

PubMed

Singh, Jitendra K; Vyas, Preeti; Dubey, Anamika; Upadhyaya, Chandrama Prakash; Kothari, Richa; Tyagi, Vineet Veer; Kumar, Ashwani

2018-06-01

The future supply of energy to meet growing energy demand of rapidly exapanding populations is based on wide energy resources, particularly the renewable ones. Among all resources, lignocellulosic biomasses such as agriculture, forest, and agro-industrial residues are the most abundant and easily available bioresource for biorefineries to provide fuels, chemicals, and materials. However, pretreatment of biomass is required to overcome the physical and chemical barriers that exist in the lignin-carbohydrate composite and pretreatment facilitate the entry of biocatalysts for the conversion of biomass into fermentable sugars and other by-products. Therefore, pretreatment of the biomass is necessary prerequisite for efficient hydrolysis of lignocelluloses into different type of fermentable sugars. The physiochemical, biochemical and biological pretreatment methods are considered as most promising technologies for the biomass hydrolysis and are discussed in this review article. We also discussed the recent advancements and modern trends in pretreatment methods of lignocelluloses conversion into ethanol with special focus on fermentation methods.

SPRUCE Pretreatment Plant Tissue Analyses, 2009 through 2013

DOE Data Explorer

Phillips, J. R. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Brice, D. J. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Hanson, P. J. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Childs, J. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Iversen, C. M. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Norby, R. J. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A; Warren, J. M. [Oak Ridge National Laboratory, U.S. Department of Energy, Oak Ridge, Tennessee, U.S.A

2009-12-01

This data set reports the results of elemental analyses of foliar and stem/woody twig plant tissues collected at the SPRUCE site in 2009, 2012, and 2013. Samples were obtained at various locations around the S1 Bog and from within the developing experimental treatment plots. These are pretreatment vegetation samples, collected prior to initiation of the SPRUCE experiment heating and elevated CO2 treatments.

The influence of different pretreatment methods on biogas production from Jatropha curcas oil cake.

PubMed

Jabłoński, Sławomir Jan; Kułażyński, Marek; Sikora, Ilona; Łukaszewicz, Marcin

2017-12-01

Drought and pest resistance, together with high oil content in its seeds, make Jatropha curcas a good oil source for biodiesel. Oil cake from J. curcas is not suitable for animal feeding and thus may be profitably used for additional energy production by conversion into biogas; however, the anaerobic digestion process must be optimized to obtain good efficiency. We subjected oil cake to thermal and acidic pretreatment to deactivate protease inhibitors and partially hydrolyze phytate. We then digested the samples in batch conditions to determine the effects of pretreatment on biogas production. Thermal pretreatment changed the kinetics of anaerobic digestion and reduced protease inhibitor activity and the concentration of phytate; however, biogas production efficiency was not affected (0.281 m 3  kg -1 ). To evaluate the possibility of recirculating water for SSF hydrolysis, ammonium nitrogen recovery from effluent was evaluated by its precipitation in the form of struvite (magnesium ammonium phosphate).Concentration of ammonium ions was reduced by 53% (to 980 mg L -1 ). We propose a water-saving concept based on percolation of J. curcas cake using anaerobic digestion effluent and feeding that percolate into a methanogenic bioreactor. Copyright © 2016 Elsevier Ltd. All rights reserved.

Anaerobic digestion of organic fraction of municipal solid waste combining two pretreatment modalities, high temperature microwave and hydrogen peroxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shahriari, Haleh, E-mail: haleh.shahriari@gmail.com; Warith, Mostafa; Hamoda, Mohamed

2012-01-15

Highlights: Black-Right-Pointing-Pointer Microwave and H{sub 2}O{sub 2} pretreatment were studied to enhance anaerobic digestion of organic waste. Black-Right-Pointing-Pointer The whole waste pretreated at 115 Degree-Sign C or 145 Degree-Sign C had the highest biogas production. Black-Right-Pointing-Pointer Biogas production of the whole waste decreased at 175 Degree-Sign C due to formation of refractory compounds. Black-Right-Pointing-Pointer Pretreatment to 145 Degree-Sign C and 175 Degree-Sign C were the best when considering only the free liquid fraction. Black-Right-Pointing-Pointer H{sub 2}O{sub 2} pretreatment had a lag phase and the biogas production was not higher than MW pretreated samples. - Abstract: In order to enhance anaerobicmore » digestion (AD) of the organic fraction of municipal solid waste (OFMSW), pretreatment combining two modalities, microwave (MW) heating in presence or absence of hydrogen peroxide (H{sub 2}O{sub 2}) were investigated. The main pretreatment variables affecting the characteristics of the OFMSW were temperature (T) via MW irradiation and supplemental water additions of 20% and 30% (SWA20 and SW30). Subsequently, the focus of this study was to evaluate mesophilic batch AD performance in terms of biogas production, as well as changes in the characteristics of the OFMSW post digestion. A high MW induced temperature range (115-175 Degree-Sign C) was applied, using sealed vessels and a bench scale MW unit equipped with temperature and pressure controls. Biochemical methane potential (BMP) tests were conducted on the whole OFMSW as well as the liquid fractions. The whole OFMSW pretreated at 115 Degree-Sign C and 145 Degree-Sign C showed 4-7% improvement in biogas production over untreated OFMSW (control). When pretreated at 175 Degree-Sign C, biogas production decreased due to formation of refractory compounds, inhibiting the digestion. For the liquid fraction of OFMSW, the effect of pretreatment on the cumulative biogas production (CBP) was more pronounced for SWA20 at 145 Degree-Sign C, with a 26% increase in biogas production after 8 days of digestion, compared to the control. When considering the increased substrate availability in the liquid fraction after MW pretreatment, a 78% improvement in biogas production vs. the control was achieved. Combining MW and H{sub 2}O{sub 2} modalities did not have a positive impact on OFMSW stabilization and enhanced biogas production. In general, all samples pretreated with H{sub 2}O{sub 2} displayed a long lag phase and the CBP was usually lower than MW irradiated only samples. First order rate constant was calculated.« less

Low severity coal liquefaction promoted by cyclic olefins. Quarterly report, January--March 1994

DOE Office of Scientific and Technical Information (OSTI.GOV)

Curtis, C.W.

Previous research has suggested that using a more effective hydrogen donor solvent in the low severity coal liquefaction reaction improves coal conversion. In order to understand the results of these methods, both independently and combined, a factorial experiment was designed. Pretreating coal with hydrochloric and sulfurous acid solutions in both water and methanol is compared with pretreating coal using only methanol and with no pretreatment. The effects of these pretreatments on coal liquefaction behavior are contrasted with the ammonium acetate pretreatment. Within each of these, individual reactions are performed with the hydroaromatic 1,2,3,4-tetrahydronaphthalene (tetralin, TET) and the cyclic olefin 1,4,5,8-tetrahydronaphthalenemore » (isotetralin, ISO). The final aspect of the factorial experiment is the comparison of Wyodak subbituminous coal (WY) from the Argonne Premium Sample Bank and Black Thunder subbituminous coal (BT) provided by Amoco. Half of the reactions in the matrix have now been completed. In all but one case, Black Thunder-HCl/H{sub 2}O, the ISO proved to be more reactive than TET. After the other four reactions using this combination are complete, the average conversion may be greater with the cyclic olefin. The second part of this paper describes the current and future work with Fourier transform infrared spectroscopy. The objective of this work is to determine the kinetics of reaction of isotetralin at high temperatures and pressures. This quarter combinations of three products typically produced from isotetralin were used in spectral subtraction.« less

[Measurement of Water COD Based on UV-Vis Spectroscopy Technology].

PubMed

Wang, Xiao-ming; Zhang, Hai-liang; Luo, Wei; Liu, Xue-mei

2016-01-01

Ultraviolet/visible (UV/Vis) spectroscopy technology was used to measure water COD. A total of 135 water samples were collected from Zhejiang province. Raw spectra with 3 different pretreatment methods (Multiplicative Scatter Correction (MSC), Standard Normal Variate (SNV) and 1st Derivatives were compared to determine the optimal pretreatment method for analysis. Spectral variable selection is an important strategy in spectrum modeling analysis, because it tends to parsimonious data representation and can lead to multivariate models with better performance. In order to simply calibration models, the preprocessed spectra were then used to select sensitive wavelengths by competitive adaptive reweighted sampling (CARS), Random frog and Successive Genetic Algorithm (GA) methods. Different numbers of sensitive wavelengths were selected by different variable selection methods with SNV preprocessing method. Partial least squares (PLS) was used to build models with the full spectra, and Extreme Learning Machine (ELM) was applied to build models with the selected wavelength variables. The overall results showed that ELM model performed better than PLS model, and the ELM model with the selected wavelengths based on CARS obtained the best results with the determination coefficient (R2), RMSEP and RPD were 0.82, 14.48 and 2.34 for prediction set. The results indicated that it was feasible to use UV/Vis with characteristic wavelengths which were obtained by CARS variable selection method, combined with ELM calibration could apply for the rapid and accurate determination of COD in aquaculture water. Moreover, this study laid the foundation for further implementation of online analysis of aquaculture water and rapid determination of other water quality parameters.

Rapid screening of illicit additives in weight loss dietary supplements with desorption corona beam ionisation (DCBI) mass spectrometry.

PubMed

Wang, H; Wu, Y; Zhao, Y; Sun, W; Ding, L; Guo, B; Chen, B

2012-08-01

Desorption corona beam ionisation (DCBI), the relatively novel ambient mass spectrometry (MS) technique, was utilised to screen for illicit additives in weight-loss food. The five usually abused chemicals - fenfluramine, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine and phenolphthalein - were detected with the proposed DCBI-MS method. Fast single-sample and high-throughput analysis was demonstrated. Semi-quantification was accomplished based on peak areas in the ion chromatograms. Four illicit additives were identified and semi-quantified in commercial samples. As there was no tedious sample pre-treatment compared with conventional HPLC methods, high-throughput analysis was achieved with DCBI. The results proved that DCBI-MS is a powerful tool for the rapid screening of illicit additives in weight-loss dietary supplements.

High-performance of Agaricus blazei fungus for the biological pretreatment of elephant grass.

PubMed

Dal Picolli, Thais; Regalin Aver, Kaliane; Claudete Fontana, Roselei; Camassola, Marli

2018-01-01

Biological pre-treatment seems to be promising being an eco-friendly process, with no inhibitor generated during the process. The potential for elephant grass pre-treatment with white degradation fungi Pleurotus ostreatus, Agaricus blazei, Lentinula edodes, Pleurotus citrinopileatus, and Pleurotus djamor, in isolated or mixed cultures of these strains, was evaluated. The highest activities of enzymes involved in the degradation of lignocellulosic biomass (laccases, endoglucanases, xylanases, and β-glucosidases) were observed for A. blazei, L. edodes and the combination of P. ostreatus and A. blazei. In the enzymatic hydrolysis, there was greater release of reducing sugars in the pre-treated elephant grass samples by A. blazei during 10 days (338.91 ± 7.39 mg g -1 of biomass). For this sample, higher lignin reductions, 24.81 and 57.45%, after 15 and 35 days of incubation, respectively, were also verified. These data indicate the potential of macromycetes such as A. blazei to perform biological pre-treatments. © 2017 American Institute of Chemical Engineers Biotechnol. Prog., 34:42-50, 2018. © 2017 American Institute of Chemical Engineers.

Hydrothermal pretreatment of microalgae for production of pyrolytic bio-oil with a low nitrogen content.

PubMed

Du, Zhenyi; Mohr, Michael; Ma, Xiaochen; Cheng, Yanling; Lin, Xiangyang; Liu, Yuhuan; Zhou, Wenguang; Chen, Paul; Ruan, Roger

2012-09-01

Microalgae can be converted to an energy-dense bio-oil via pyrolysis; however, the relatively high nitrogen content of this bio-oil presents a challenge for its direct use as fuels. Therefore, hydrothermal pretreatment was employed to reduce the N content in Nannochloropsis oculata feedstock by removing proteins without requiring significant energy inputs. The effects of reaction conditions on the yield and composition of pretreated algae were investigated by varying the temperature (150-225°C) and reaction time (10-60 min). Compared with untreated algae, pretreated samples had higher carbon contents and enhanced heating values under all reaction conditions and 6-42% lower N contents at 200-225°C for 30-60 min. The pyrolytic bio-oil from pretreated algae contained less N-containing compounds than that from untreated samples and the bio-oil contained mainly (44.9% GC-MS peak area) long-chain fatty acids (C14-C18) which can be more readily converted into hydrocarbon fuels in the presence of simple catalysts. Copyright © 2012 Elsevier Ltd. All rights reserved.

Combined pretreatment with hot compressed water and wet disk milling opened up oil palm biomass structure resulting in enhanced enzymatic digestibility.

PubMed

Zakaria, Mohd Rafein; Hirata, Satoshi; Fujimoto, Shinji; Hassan, Mohd Ali

2015-10-01

Combined pretreatment with hot compressed water and wet disk milling was performed with the aim to reduce the natural recalcitrance of oil palm biomass by opening its structure and provide maximal access to cellulase attack. Oil palm empty fruit bunch and oil palm frond fiber were first hydrothermally pretreated at 150-190° C and 10-240 min. Further treatment with wet disk milling resulted in nanofibrillation of fiber which caused the loosening of the tight biomass structure, thus increasing the subsequent enzymatic conversion of cellulose to glucose. The effectiveness of the combined pretreatments was evaluated by chemical composition changes, power consumption, morphological alterations by SEM and the enzymatic digestibility of treated samples. At optimal pretreatment process, approximately 88.5% and 100.0% of total sugar yields were obtained from oil palm empty fruit bunch and oil palm frond fiber samples, which only consumed about 15.1 and 23.5 MJ/kg of biomass, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Two-step sequential pretreatment for the enhanced enzymatic hydrolysis of coffee spent waste.

PubMed

Ravindran, Rajeev; Jaiswal, Swarna; Abu-Ghannam, Nissreen; Jaiswal, Amit K

2017-09-01

In the present study, eight different pretreatments of varying nature (physical, chemical and physico-chemical) followed by a sequential, combinatorial pretreatment strategy was applied to spent coffee waste to attain maximum sugar yield. Pretreated samples were analysed for total reducing sugar, individual sugars and generation of inhibitory compounds such as furfural and hydroxymethyl furfural (HMF) which can hinder microbial growth and enzyme activity. Native spent coffee waste was high in hemicellulose content. Galactose was found to be the predominant sugar in spent coffee waste. Results showed that sequential pretreatment yielded 350.12mg of reducing sugar/g of substrate, which was 1.7-fold higher than in native spent coffee waste (203.4mg/g of substrate). Furthermore, extensive delignification was achieved using sequential pretreatment strategy. XRD, FTIR, and DSC profiles of the pretreated substrates were studied to analyse the various changes incurred in sequentially pretreated spent coffee waste as opposed to native spent coffee waste. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of pretreatments on biogas production from microalgae biomass grown in pig manure treatment plants.

PubMed

Martín Juárez, Judit; Riol Pastor, Elena; Fernández Sevilla, José M; Muñoz Torre, Raúl; García-Encina, Pedro A; Bolado Rodríguez, Silvia

2018-06-01

Methane production from pretreated and raw mixed microalgae biomass grown in pig manure was evaluated. Acid and basic pretreatments provided the highest volatile solids solubilisation (up to 81%) followed by alkaline-peroxide and ultrasounds (23%). Bead milling and steam explosion remarkably increased the methane production rate, although the highest yield (377 mL CH 4 /g SV) was achieved by alkali pretreatment. Nevertheless, some pretreatments inhibited biogas production and resulted in lag phases of 7-9 days. Hence, experiments using only the pretreated solid phase were performed, which resulted in a decrease in the lag phase to 2-3 days for the alkali pretreatment and slightly increased biomass biodegradability of few samples. The limiting step during the BMP test (hydrolysis or microbial inhibition) for each pretreatment was elucidated using the goodness of fitting to a first order or a Gompertz model. Finally, the use of digestate as biofertilizer was evaluated applying a biorefinery concept. Copyright © 2018 Elsevier Ltd. All rights reserved.

Disruption of Membranes of Extracellular Vesicles Is Necessary for ELISA Determination of Urine AQP2: Proof of Disruption and Epitopes of AQP2 Antibodies

PubMed Central

Nameta, Masaaki; Saijo, Yoko; Ohmoto, Yasukazu; Katsuragi, Kiyonori; Yamamoto, Keiko; Yamamoto, Tadashi; Ishibashi, Kenichi; Sasaki, Sei

2016-01-01

Aquaporin-2 (AQP2) is present in urine extracellular vesicles (EVs) and is a useful biomarker for water balance disorders. We previously found that pre-treatment of urine with alkali/detergent or storage at −25 °C is required for enzyme-linked immunosorbent assay (ELISA) measurement. We speculated that disruptions of EVs membranes are necessary to allow for the direct contact of antibodies with their epitopes. Human urine EVs were prepared using an ultracentrifugation method. Urine EV samples were stored at different temperatures for a week. Electron microscopy showed abundant EVs with diameters of 20–100 nm, consistent with those of exosomes, in normal urine, whereas samples from alkali/detergent pre-treated urine showed fewer EVs with large swollen shapes and frequent membrane disruptions. The abundance and structures of EVs were maintained during storage at −80 °C, but were severely damaged at −25 °C. Binding and competitive inhibition assays showed that epitopes of monoclonal antibody and polyclonal antibody were the hydrophilic Loop D and C-terminus of AQP2, respectively, both of which are present on the inner surface of EVs. Thus, urine storage at −25 °C or pre-treatment with alkali/detergent disrupt EVs membranes and allow AQP2 antibodies to bind to their epitopes located inside EVs. PMID:27681727

Multimodal analysis of pretreated biomass species highlights generic markers of lignocellulose recalcitrance.

PubMed

Herbaut, Mickaël; Zoghlami, Aya; Habrant, Anouck; Falourd, Xavier; Foucat, Loïc; Chabbert, Brigitte; Paës, Gabriel

2018-01-01

Biomass recalcitrance to enzymatic hydrolysis has been assigned to several structural and chemical factors. However, their relative importance remains challenging to evaluate. Three representative biomass species (wheat straw, poplar and miscanthus) were submitted to four standard pretreatments (dilute acid, hot water, ionic liquid and sodium chlorite) in order to generate a set of contrasted samples. A large array of techniques, including wet chemistry analysis, porosity measurements using NMR spectroscopy, electron and fluorescence microscopy, were used in order to determine possible generic factors of biomass recalcitrance. The pretreatment conditions selected allowed obtaining samples displaying different susceptibility to enzymatic hydrolysis (from 3 up to 98% of the initial glucose content released after 96 h of saccharification). Generic correlation coefficients were calculated between the measured chemical and structural features and the final saccharification rates. Increases in porosity displayed overall strong positive correlations with saccharification efficiency, but different porosity ranges were concerned depending on the considered biomass. Lignin-related factors displayed highly negative coefficients for all biomasses. Lignin content, which is likely involved in the correlations observed for porosity, was less detrimental to enzymatic hydrolysis than lignin composition. Lignin influence was highlighted by the strong negative correlation with fluorescence intensity which mainly originates from monolignols in mature tissues. Our results provide a better understanding of the factors responsible for biomass recalcitrance that can reasonably be considered as generic. The correlations with specific porosity ranges are biomass species-dependent, meaning that enzymes cocktails with fitted enzyme size are likely to be needed to optimise saccharification depending on the biomass origin. Lignin composition, which probably influences its structure, is the most important parameter to overcome to enhance enzymes access to the polysaccharides. Accordingly, fluorescence intensity was found to be a rapid and simple method to assess recalcitrance after pretreatment.

Bioanalytical challenge: A review of environmental and pharmaceuticals contaminants in human milk.

PubMed

Lopes, Bianca Rebelo; Barreiro, Juliana Cristina; Cass, Quezia Bezerra

2016-10-25

An overview of bioanalytical methods for the determination of environmental and pharmaceutical contaminants in human milk is presented. The exposure of children to these contaminants through lactation has been widely investigated. The human milk contains diverse proteins, lipids, and carbohydrates and the concentration of these components is drastically altered during the lactation period providing a high degree of an analytical challenge. Sample collection and pretreatment are still considered the Achilles' heel. This review presents liquid chromatographic methods developed in the last 10 years for this complex matrix with focuses in the extraction and quantification steps. Green sample preparation protocols have been emphasized. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of aqueous ammonia and dilute acid pretreatment of bamboo fractions: Structure properties and enzymatic hydrolysis.

PubMed

Xin, Donglin; Yang, Zhong; Liu, Feng; Xu, Xueru; Zhang, Junhua

2015-01-01

The effect of two pretreatments methods, aqueous ammonia (SAA) and dilute acid (DA), on the chemical compositions, cellulose crystallinity, morphologic change, and enzymatic hydrolysis of bamboo fractions (bamboo yellow, timber, green, and knot) was compared. Bamboo fractions with SAA pretreatment had better hydrolysability than those with DA pretreatment. High crystallinity index resulted in low hydrolysis yield in the conversion of SAA pretreated bamboo fractions, not DA pretreated fractions. The increase of cellulase loading had modestly positive effect in the hydrolysis of both SAA and DA pretreated bamboo fractions, while supplement of xylanase significantly increased the hydrolysis of the pretreated bamboo fractions, especially after SAA pretreatment. The results indicated that SAA pretreatment was more effective than DA pretreatment in conversion of bamboo fractions, and supplementation of xylanase was necessary in effective conversion of the SAA pretreated fractions into fermentable sugars. Copyright © 2014 Elsevier Ltd. All rights reserved.

Positive lists of cosmetic ingredients: Analytical methodology for regulatory and safety controls - A review.

PubMed

Lores, Marta; Llompart, Maria; Alvarez-Rivera, Gerardo; Guerra, Eugenia; Vila, Marlene; Celeiro, Maria; Lamas, J Pablo; Garcia-Jares, Carmen

2016-04-07

Cosmetic products placed on the market and their ingredients, must be safe under reasonable conditions of use, in accordance to the current legislation. Therefore, regulated and allowed chemical substances must meet the regulatory criteria to be used as ingredients in cosmetics and personal care products, and adequate analytical methodology is needed to evaluate the degree of compliance. This article reviews the most recent methods (2005-2015) used for the extraction and the analytical determination of the ingredients included in the positive lists of the European Regulation of Cosmetic Products (EC 1223/2009): comprising colorants, preservatives and UV filters. It summarizes the analytical properties of the most relevant analytical methods along with the possibilities of fulfilment of the current regulatory issues. The cosmetic legislation is frequently being updated; consequently, the analytical methodology must be constantly revised and improved to meet safety requirements. The article highlights the most important advances in analytical methodology for cosmetics control, both in relation to the sample pretreatment and extraction and the different instrumental approaches developed to solve this challenge. Cosmetics are complex samples, and most of them require a sample pretreatment before analysis. In the last times, the research conducted covering this aspect, tended to the use of green extraction and microextraction techniques. Analytical methods were generally based on liquid chromatography with UV detection, and gas and liquid chromatographic techniques hyphenated with single or tandem mass spectrometry; but some interesting proposals based on electrophoresis have also been reported, together with some electroanalytical approaches. Regarding the number of ingredients considered for analytical control, single analyte methods have been proposed, although the most useful ones in the real life cosmetic analysis are the multianalyte approaches. Copyright © 2016 Elsevier B.V. All rights reserved.

Pretreatment of food waste with high voltage pulse discharge towards methane production enhancement.

PubMed

Zou, Lianpei; Ma, Chaonan; Liu, Jianyong; Li, Mingfei; Ye, Min; Qian, Guangren

2016-12-01

Anaerobic batch tests were performed to investigate the methane production enhancement and solid transformation rates from food waste (FW) by high voltage pulse discharge (HVPD) pretreatment. The total cumulative methane production with HVPD pretreatment was 134% higher than that of the control. The final volatile solids transformation rates of FW with and without HVPD pretreatment were 54.3% and 32.3%, respectively. Comparison study on HVPD pretreatment with acid, alkali and ultrasonic pretreatments showed that the methane production and COD removal rates of FW pretreated with HVPD were more than 100% higher than the control, but only about 50% higher can be obtained with other pretreatments. HVPD pretreatment could be a promising pretreatment method in the application of energy recovery from FW. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microwave-assisted co-pyrolysis of pretreated lignin and soapstock for upgrading liquid oil: Effect of pretreatment parameters on pyrolysis behavior.

PubMed

Duan, Dengle; Ruan, Roger; Lei, Hanwu; Liu, Yuhuan; Wang, Yunpu; Zhang, Yayun; Zhao, Yunfeng; Dai, Leilei; Wu, Qiuhao; Zhang, Shumei

2018-06-01

The co-pyrolysis of pretreated lignin and soapstock was carried out to upgrade vapors under microwave irradiation. Results showed that the yield of 29.92-42.21 wt% of upgraded liquid oil was achieved under varied pretreatment conditions. Char yield decreased from 32.44 wt% for untreated control to 24.35 wt% for the 150 °C pretreated samples. The increased temperature, irradiation time and acid concentration were conducive to decrease the relative contents of phenols and oxygenates in liquid oils. The main components of the liquid oil were gasoline fraction (mono-aromatics and C5-C12 aliphatics), which ranged from 57.38 to 71.98% under various pretreatment conditions. Meanwhile, the diesel fraction (C12+ aliphatics) ranged from 13.16 to 22.62% from co-pyrolysis of pretreated lignin and soapstock, comparing with 10.18% of C12+ aliphatics from co-pyrolysis of non-pretreated lignin and soapstock. A possible mechanism was proposed for co-pyrolysis of pretreated lignin and soapstock for upgraded liquid oils. Copyright © 2018 Elsevier Ltd. All rights reserved.

Effect of Varying Acid Hydrolysis Condition in Gracilaria Sp. Fermentation Using Sasad

NASA Astrophysics Data System (ADS)

Mansuit, H.; Samsuri, M. D. C.; Sipaut, C. S.; Yee, C. F.; Yasir, S. M.; Mansa, R.

2015-04-01

Macroalgae or seaweed is being considered as promising feedstock for bioalcohol production due to high polysaccharides content. Polysaccharides can be converted into fermentable sugar through acid hydrolysis pre-treatment. In this study, the potential of using carbohydrate-rich macroalgae, Gracilaria sp. as feedstock for bioalcohol production via various acid hydrolysis conditions prior to the fermentation process was investigated and evaluated. The seaweed used in this research was from the red algae group, using species of Gracilaria sp. which was collected from Sg. Petani Kedah, Malaysia. Pre-treatment of substrate was done using H2SO4 and HCl with molarity ranging from 0.2M to 0.8M. The pretreatment time were varied in the range of 15 to 30 minutes. Fermentation was conducted using Sasad, a local Sabahan fermentation agent as a starter culture. Alcohol extraction was done using a distillation unit. Reducing sugar analysis was done by Benedict test method. Alcohol content analysis was done using specific gravity test. After hydrolysis, it was found out that acid hydrolysis at 0.2M H2SO4 and pre-treated for 20 minutes at 121°C has shown the highest reducing sugar content which has yield (10.06 mg/g) of reducing sugar. It was followed by other samples hydrolysis using 0.4M HCl with 30 minutes pre-treatment and 0.2M H2SO4, 15 minutes pre-treatment with yield of 8.06 mg/g and 5.75 mg/g reducing sugar content respectively. In conclusion, acid hydrolysis of Gracilaria sp. can produce higher reducing sugar yield and thus it can further enhance the bioalcohol production yield. Hence, acid hydrolysis of Gracilaria sp. should be studied more as it is an important step in the bioalcohol production and upscaling process.

Frontiers of Two-Dimensional Correlation Spectroscopy. Part 1. New concepts and noteworthy developments

NASA Astrophysics Data System (ADS)

Noda, Isao

2014-07-01

A comprehensive survey review of new and noteworthy developments, which are advancing forward the frontiers in the field of 2D correlation spectroscopy during the last four years, is compiled. This review covers books, proceedings, and review articles published on 2D correlation spectroscopy, a number of significant conceptual developments in the field, data pretreatment methods and other pertinent topics, as well as patent and publication trends and citation activities. Developments discussed include projection 2D correlation analysis, concatenated 2D correlation, and correlation under multiple perturbation effects, as well as orthogonal sample design, predicting 2D correlation spectra, manipulating and comparing 2D spectra, correlation strategy based on segmented data blocks, such as moving-window analysis, features like determination of sequential order and enhanced spectral resolution, statistical 2D spectroscopy using covariance and other statistical metrics, hetero-correlation analysis, and sample-sample correlation technique. Data pretreatment operations prior to 2D correlation analysis are discussed, including the correction for physical effects, background and baseline subtraction, selection of reference spectrum, normalization and scaling of data, derivatives spectra and deconvolution technique, and smoothing and noise reduction. Other pertinent topics include chemometrics and statistical considerations, peak position shift phenomena, variable sampling increments, computation and software, display schemes, such as color coded format, slice and power spectra, tabulation, and other schemes.

Methane yield in source-sorted organic fraction of municipal solid waste.

PubMed

Davidsson, Asa; Gruvberger, Christopher; Christensen, Thomas H; Hansen, Trine Lund; Jansen, Jes la Cour

2007-01-01

Treating the source-separated organic fraction of municipal solid waste (SS-OFMSW) by anaerobic digestion is considered by many municipalities in Europe as an environmentally friendly means of treating organic waste and simultaneously producing methane gas. Methane yield can be used as a parameter for evaluation of the many different systems that exist for sorting and pre-treating waste. Methane yield from the thermophilic pilot scale digestion of 17 types of domestically SS-OFMSW originating from seven full-scale sorting systems was found. The samples were collected during 1 year using worked-out procedures tested statistically to ensure representative samples. Each waste type was identified by its origin and by pre-sorting, collection and pre-treatment methods. In addition to the pilot scale digestion, all samples were examined by chemical analyses and methane potential measurements. A VS-degradation rate of around 80% and a methane yield of 300-400Nm(3) CH(4)/ton VS(in) were achieved with a retention time of 15 days, corresponding to approximately 70% of the methane potential. The different waste samples gave minor variation in chemical composition and thus also in methane yield and methane potential. This indicates that sorting and collection systems in the present study do not significantly affect the amount of methane produced per VS treated.

A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

PubMed

Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

2017-07-01

As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% (n=3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison between solid-state and powder-state alkali pretreatment on saccharification and fermentation for bioethanol production from rice straw.

PubMed

Yeasmin, Shabina; Kim, Chul-Hwan; Islam, Shah Md Asraful; Lee, Ji-Young

2016-01-01

The efficacy of different concentrations of NaOH (0.25%, 0.50%, 0.75%, and 1.00%) for the pretreatment of rice straw in solid and powder state in enzymatic saccharification and fermentation for the production of bioethanol was evaluated. A greater amount of biomass was recovered through solid-state pretreatment (3.74 g) from 5 g of rice straw. The highest increase in the volume of rice straw powder as a result of swelling was observed with 1.00% NaOH pretreatment (48.07%), which was statistically identical to 0.75% NaOH pretreatment (32.31%). The surface of rice straw was disrupted by the 0.75% NaOH and 1.00% NaOH pretreated samples as observed using field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). In Fourier-transform infrared (FT-IR) spectra, absorbance of hydroxyl groups at 1,050 cm(-1) due to the OH group of lignin was gradually decreased with the increase of NaOH concentration. The greatest amounts of glucose and ethanol were obtained in 1.00% NaOH solid-state pretreated and powder-state hydrolyzed samples (0.804 g g(-1) and 0.379 g g(-1), respectively), which was statistically similar to the use of 0.75% NaOH (0.763 g g(-1) and 0.358 g g(-1), respectively). Thus, solid-state pretreatment with 0.75% NaOH and powder-state hydrolysis appear to be suitable for fermentation and bioethanol production from rice straw.

Determination of alcohol and extract concentration in beer samples using a combined method of near-infrared (NIR) spectroscopy and refractometry.

PubMed

Castritius, Stefan; Kron, Alexander; Schäfer, Thomas; Rädle, Matthias; Harms, Diedrich

2010-12-22

A new approach of combination of near-infrared (NIR) spectroscopy and refractometry was developed in this work to determine the concentration of alcohol and real extract in various beer samples. A partial least-squares (PLS) regression, as multivariate calibration method, was used to evaluate the correlation between the data of spectroscopy/refractometry and alcohol/extract concentration. This multivariate combination of spectroscopy and refractometry enhanced the precision in the determination of alcohol, compared to single spectroscopy measurements, due to the effect of high extract concentration on the spectral data, especially of nonalcoholic beer samples. For NIR calibration, two mathematical pretreatments (first-order derivation and linear baseline correction) were applied to eliminate light scattering effects. A sample grouping of the refractometry data was also applied to increase the accuracy of the determined concentration. The root mean squared errors of validation (RMSEV) of the validation process concerning alcohol and extract concentration were 0.23 Mas% (method A), 0.12 Mas% (method B), and 0.19 Mas% (method C) and 0.11 Mas% (method A), 0.11 Mas% (method B), and 0.11 Mas% (method C), respectively.

Removal of uranium from soil samples for ICP-OES analysis of RCRA metals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wero, M.; Lederer-Cano, A.; Billy, C.

1995-12-01

Soil samples containing high levels of uranium present unique analytical problems when analyzed for toxic metals (Ag, As, Ba, Cd, Cr, Cu, Ni, Pb, Se and Tl) because of the spectral interference of uranium in the ICP-OES emission spectrometer. Methods to remove uranium from the digestates of soil samples, known to be high in uranium, have been developed that reduce the initial uranium concentration (1-3%) to less than 500 ppm. UTEVA ion exchange columns, used as an ICP-OES analytical pre-treatment, reduces uranium to acceptable levels, permitting good analytical results of the RCRA metals by ICP-OES.

Effect of chemical pretreatments on corn stalk bagasse as immobilizing carrier of Clostridium acetobutylicum in the performance of a fermentation-pervaporation coupled system.

PubMed

Cai, Di; Li, Ping; Chen, Changjing; Wang, Yong; Hu, Song; Cui, Caixia; Qin, Peiyong; Tan, Tianwei

2016-11-01

In this study, different pretreatment methods were evaluated for modified the corn stalk bagasse and further used the pretreated bagasse as immobilized carrier in acetone-butanol-ethanol fermentation process. Structural changes of the bagasses pretreated by different methods were analyzed by Fourier transform infrared, crystallinity index and scanning pictures by electron microscope. And the performances of batch fermentation using the corn stalk based carriers were evaluated. Results indicated that the highest ABE concentration of 23.86g/L was achieved using NaOH pretreated carrier in batch fermentation. Immobilized fermentation-pervaporation integration process was further carried out. The integration process showed long-term stability with 225-394g/L of ABE solvents on the permeate side of pervaporation membrane. This novel integration process was found to be an efficient method for biobutanol production. Copyright © 2016 Elsevier Ltd. All rights reserved.

A procedure for partitioning bulk sediments into distinct grain-size fractions for geochemical analysis

USGS Publications Warehouse

Barbanti, A.; Bothner, Michael H.

1993-01-01

A method to separate sediments into discrete size fractions for geochemical analysis has been tested. The procedures were chosen to minimize the destruction or formation of aggregates and involved gentle sieving and settling of wet samples. Freeze-drying and sonication pretreatments, known to influence aggregates, were used for comparison. Freeze-drying was found to increase the silt/clay ratio by an average of 180 percent compared to analysis of a wet sample that had been wet sieved only. Sonication of a wet sample decreased the silt/clay ratio by 51 percent. The concentrations of metals and organic carbon in the separated fractions changed depending on the pretreatment procedures in a manner consistent with the hypothesis that aggregates consist of fine-grained organic- and metal-rich particles. The coarse silt fraction of a freeze-dried sample contained 20–44 percent higher concentrations of Zn, Cu, and organic carbon than the coarse silt fraction of the wet sample. Sonication resulted in concentrations of these analytes that were 18–33 percent lower in the coarse silt fraction than found in the wet sample. Sonication increased the concentration of lead in the clay fraction by an average of 40 percent compared to an unsonicated sample. Understanding the magnitude of change caused by different analysis protocols is an aid in designing future studies that seek to interpret the spatial distribution of contaminated sediments and their transport mechanisms.

Effects of different freezing methods on calcium enriched papaya (Carica papaya L.).

PubMed

Lovera, Nancy N; Ramallo, Laura; Salvadori, Viviana O

2018-06-01

The effect of calcium impregnation on drip loss, colour, mechanical properties, sensory perception and freezing time on frozen-thawed papaya was studied, evaluating different freezing methods: cryogenic, tunnel and household freezer freezing. Osmotic dehydration as pre-treatment was also evaluated. Freezing in liquid nitrogen was considered an inappropriate method for papaya preservation due to cracking. Calcium impregnation and osmotic dehydration increased tissue firmness and decreased freezing time (freezing time for fresh, calcium impregnated and osmo-dehydrated fruit was 23, 17 and 5 min in a tunnel and 118, 83 and 60 min in a household freezer, respectively). Calcium lactate was the most effective way to protect tissue's firmness before and after a freeze-thaw cycle (maximum stress values approx. 300-400% of the raw tissue for tunnel freezing and 260% for household freezer). Microstructure analysis showed better tissue integrity retention in papaya samples impregnated with calcium lactate than in those with calcium gluconate, after a freezing-thawing cycle, in agreement with the drip loss results. In spite of these results, consumers preferred frozen papaya without pre-treatment or impregnated with calcium gluconate.

Analysis of volatile compounds by open-air ionization mass spectrometry.

PubMed

Meher, Anil Kumar; Chen, Yu-Chie

2017-05-08

This study demonstrates a simple method for rapid and in situ identification of volatile and endogenous compounds in culinary spice samples through mass spectrometry (MS). This method only requires a holder for solid spice sample (2-3 mm) that is placed close to a mass spectrometer inlet, which is applied with a high voltage. Volatile species responsible for the aroma of the spice samples can be readily detected by the mass spectrometer. Sample pretreatment is not required prior to MS analysis, and no solvent was used during MS analysis. The high voltage applied to the inlet of the mass spectrometer induces the ionization of volatile compounds released from the solid spice samples. Furthermore, moisture in the air also contributes to the ionization of volatile compounds. Dried spices including cinnamon and cloves are used as the model sample to demonstrate this straightforward MS analysis, which can be completed within few seconds. Furthermore, we also demonstrate the suitability of the current method for rapid screening of cinnamon quality through detection of the presence of a hepatotoxic agent, i.e. coumarin. Copyright © 2017 Elsevier B.V. All rights reserved.

Pretreatment of Lignocellulosic Wastes to Improve Ethanol and Biogas Production: A Review

PubMed Central

Taherzadeh, Mohammad J.; Karimi, Keikhosro

2008-01-01

Lignocelluloses are often a major or sometimes the sole components of different waste streams from various industries, forestry, agriculture and municipalities. Hydrolysis of these materials is the first step for either digestion to biogas (methane) or fermentation to ethanol. However, enzymatic hydrolysis of lignocelluloses with no pretreatment is usually not so effective because of high stability of the materials to enzymatic or bacterial attacks. The present work is dedicated to reviewing the methods that have been studied for pretreatment of lignocellulosic wastes for conversion to ethanol or biogas. Effective parameters in pretreatment of lignocelluloses, such as crystallinity, accessible surface area, and protection by lignin and hemicellulose are described first. Then, several pretreatment methods are discussed and their effects on improvement in ethanol and/or biogas production are described. They include milling, irradiation, microwave, steam explosion, ammonia fiber explosion (AFEX), supercritical CO2 and its explosion, alkaline hydrolysis, liquid hot-water pretreatment, organosolv processes, wet oxidation, ozonolysis, dilute-and concentrated-acid hydrolyses, and biological pretreatments. PMID:19325822

Improving methane production from digested manure biofibers by mechanical and thermal alkaline pretreatment.

PubMed

Tsapekos, P; Kougias, Panagiotis G; Frison, A; Raga, R; Angelidaki, I

2016-09-01

Animal manure digestion is associated with limited methane production, due to the high content in fibers, which are hardly degradable lignocellulosic compounds. In this study, different mechanical and thermal alkaline pretreatment methods were applied to partially degradable fibers, separated from the effluent stream of biogas reactors. Batch and continuous experiments were conducted to evaluate the efficiency of these pretreatments. In batch experiments, the mechanical pretreatment improved the degradability up to 45%. Even higher efficiency was shown by applying thermal alkaline pretreatments, enhancing fibers degradability by more than 4-fold. In continuous experiments, the thermal alkaline pretreatment, using 6% NaOH at 55°C was proven to be the most efficient pretreatment method as the methane production was increased by 26%. The findings demonstrated that the methane production of the biogas plants can be increased by further exploiting the fraction of the digested manure fibers which are discarded in the post-storage tank. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effects of Microgravity on Embryonic Quail Eye Development

NASA Technical Reports Server (NTRS)

Barrett, Joyce E.; Wells, Diane C.; Paulsen, Avelina Q.; Conrad, Gary W.

1997-01-01

Immunohistochemical methods were used to stain neurofilament protein in corneal nerves of Embryonic Day 16 (E16) quail eyes that had been fixed in 4% paraformaldehyde at room temperature for several months. Fixation was according to the methods used by the Mir 21/NASA 2 Avian Developmental Biology Flight Experiments for quail embryos incubated on the Mir Space Station. After fixation, corneas were pretreated to improve immunohistochemical visualization of neurofilaments. A sequential combination of three pretreatments [microwave heating in saline G, followed by extraction with sodium dodecyl sulfate (SDS) at 37 C, followed by digestion with hyaluronidase at 37 C], produced increased antibody staining of corneal nerve neurofilament proteins, compared with corneas subjected to no prior pretreatments. Darker nerve staining and increased numbers of fine branches were observed, together with lower background staining after such pretreatments. In contrast, use of any single pretreatment or pair of pretreatments resulted in only slight and inconsistent enhancement of nerve staining. Only the sequential combination of all three pretreatments resulted in consistently better nerve staining.

Centrifuge-less dispersive liquid-liquid microextraction base on the solidification of switchable solvent for rapid on-site extraction of four pyrethroid insecticides in water samples.

PubMed

Hu, Lu; Wang, Huazi; Qian, Heng; Liu, Chaoran; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Xu, Donghui

2016-11-11

An on-site dispersive liquid liquid microextraction base on the solidification of switchable solvent has been developed as a simple, rapid and eco-friendly sample extraction method for the fast determination of pyrethroid insecticides in aqueous samples using high-performance liquid chromatography with ultraviolet detection. In this extraction method, medium-chain saturated fatty acids (n≥10), which can rapidly solidify at low temperatures (<20°C), were investigated as switchable hydrophilic solvents. The fatty acids were converted into the hydrophilic form by adding sodium hydroxide. Microdroplets of the fatty acids were generated when injected into an acidic sample that had been pretreated by the addition of sulfuric acid. The formed cloudy solution was cooled to a low temperature to turn the fatty acids into a solid, which was then separated by filtration, thus avoiding the time-consuming step of centrifugation. The microextraction process was performed in a 10mL syringe and the pretreatment process could thus be finished in 5min. No external energy resources were required in this method, which makes it a potential method for on-site extraction. The optimal experimental parameters were as follows: 350μL of decanoic acid (1mol/L) was used as the extraction solvent, 150μL of sulfuric acid (2mol/L) was used to decrease the pH of the samples, no salt was added, and the temperature of the samples was in the range of 20-40°C. Finally, the sample was cooled in an ice bath for three minutes. Under these optimal conditions, good responses for four pyrethroid insecticides were obtained in the concentration ranges of 1-500μg/L, with coefficients of determination greater than 0.9993. The recoveries of the four pyrethroid insecticides ranged from 84.7 to 95.3%, with relative standard deviations ranging from 1.6 to 4.6%. The limits of detection based on a signal-to-noise ratio of 3 were in the range of 0.24-0.68μg/L, and the enrichment factors were in the range of 121-136. The results demonstrate that this method was successfully applied to determine pyrethroid insecticides in real water samples. No centrifugation or any special apparatus are required, make this a promising method for rapid field-sampling procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

Asparagus stem as a new lignocellulosic biomass feedstock for anaerobic digestion: increasing hydrolysis rate, methane production and biodegradability by alkaline pretreatment.

PubMed

Chen, Xiaohua; Gu, Yu; Zhou, Xuefei; Zhang, Yalei

2014-07-01

Recently, anaerobic digestion of lignocellulosic biomass for methane production has attracted considerable attention. However, there is little information regarding methane production from asparagus stem, a typical lignocellulosic biomass, by anaerobic digestion. In this study, alkaline pretreatment of asparagus stem was investigated for its ability to increase hydrolysis rate and methane production and to improve biodegradability (BD). The hydrolysis rate increased with increasing NaOH dose, due to higher removal rates of lignin and hemicelluloses. However, the optimal NaOH dose was 6% (w/w) according to the specific methane production (SMP). Under this condition, the SMP and the technical digestion time of the NaOH-treated asparagus stem were 242.3 mL/g VS and 18 days, which were 38.4% higher and 51.4% shorter than those of the untreated sample, respectively. The BD was improved from 40.1% to 55.4%. These results indicate that alkaline pretreatment could be an efficient method for increasing methane production from asparagus stem. Copyright © 2014 Elsevier Ltd. All rights reserved.

Seeing biomass recalcitrance through fluorescence.

PubMed

Auxenfans, Thomas; Terryn, Christine; Paës, Gabriel

2017-08-18

Lignocellulosic biomass is the only renewable carbon resource available in sufficient amount on Earth to go beyond the fossil-based carbon economy. Its transformation requires controlled breakdown of polymers into a set of molecules to make fuels, chemicals and materials. But biomass is a network of various inter-connected polymers which are very difficult to deconstruct optimally. In particular, saccharification potential of lignocellulosic biomass depends on several complex chemical and physical factors. For the first time, an easily measurable fluorescence properties of steam-exploded biomass samples from miscanthus, poplar and wheat straw was shown to be directly correlated to their saccharification potential. Fluorescence can thus be advantageously used as a predictive method of biomass saccharification. The loss in fluorescence occurring after the steam explosion pretreatment and increasing with pretreatment severity does not originate from the loss in lignin content, but rather from a decrease of the lignin β-aryl-ether linkage content. Fluorescence lifetime analysis demonstrates that monolignols making lignin become highly conjugated after steam explosion pretreatment. These results reveal that lignin chemical composition is a more important feature to consider than its content to understand and to predict biomass saccharification.

Investigation of irradiated rats DNA in the presence of Cu(II) chelates of amino acids Schiff bases.

PubMed

Karapetyan, N H; Torosyan, A L; Malakyan, M; Bajinyan, S A; Haroutiunian, S G

2016-01-01

The new synthesized Cu(II) chelates of amino acids Schiff bases were studied as a potential radioprotectors. Male albino rats of Wistar strain were exposed to X-ray whole-body irradiation at 4.8 Gy. This dose caused 30% mortality of the animals (LD30). The survival of animals exposed to radiation after preliminary administration of 10 mg/kg Cu(II)(Nicotinyl-L-Tyrosinate)2 or Cu(II)(Nicotinyl-L-Tryptophanate)2 prior to irradiation was registered about 80 and 100% correspondingly. Using spectrophotometric melting and agarose gel electrophoresis methods, the differences between the DNA isolated from irradiated rats and rats pretreated with Cu(II) chelates were studied. The fragments of DNA with different breaks were revealed in DNA samples isolated from irradiated animals. While, the repair of the DNA structure was observed for animals pretreated with the Cu(II) chelates. The results suggested that pretreatment of the irradiated rats with Cu(II)(Nicotinyl-L-Tyrosinate)2 and Cu(II)(Nicotinyl-L-Tryptophanate)2 compounds improves the liver DNA characteristics.

Method and apparatus for gasifying with a fluidized bed gasifier having integrated pretreating facilities

DOEpatents

Rice, Louis F.

1981-01-01

An integral gasifier including a pretreater section and a gasifier section separated by a distribution grid is defined by a single vessel. The pretreater section pretreats coal or other carbon-containing material to be gasified to prevent caking and agglomeration of the coal in the gasifier. The level of the coal bed of the pretreater section and thus the holding or residence time in said bed is selectively regulated by the amount of pretreated coal which is lifted up a lift pipe into the gasifier section. Thus, the holding time in the pretreater section can be varied according to the amount of pretreat necessary for the particular coal to be gasified.

Validated ¹H and 13C Nuclear Magnetic Resonance Methods for the Quantitative Determination of Glycerol in Drug Injections.

PubMed

Lu, Jiaxi; Wang, Pengli; Wang, Qiuying; Wang, Yanan; Jiang, Miaomiao

2018-05-15

In the current study, we employed high-resolution proton and carbon nuclear magnetic resonance spectroscopy (¹H and 13 C NMR) for quantitative analysis of glycerol in drug injections without any complex pre-treatment or derivatization on samples. The established methods were validated with good specificity, linearity, accuracy, precision, stability, and repeatability. Our results revealed that the contents of glycerol were convenient to calculate directly via the integration ratios of peak areas with an internal standard in ¹H NMR spectra, while the integration of peak heights were proper for 13 C NMR in combination with an external calibration of glycerol. The developed methods were both successfully applied in drug injections. Quantitative NMR methods showed an extensive prospect for glycerol determination in various liquid samples.

NK sensitivity of neuroblastoma cells determined by a highly sensitive coupled luminescent method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ogbomo, Henry; Hahn, Anke; Geiler, Janina

2006-01-06

The measurement of natural killer (NK) cells toxicity against tumor or virus-infected cells especially in cases with small blood samples requires highly sensitive methods. Here, a coupled luminescent method (CLM) based on glyceraldehyde-3-phosphate dehydrogenase release from injured target cells was used to evaluate the cytotoxicity of interleukin-2 activated NK cells against neuroblastoma cell lines. In contrast to most other methods, CLM does not require the pretreatment of target cells with labeling substances which could be toxic or radioactive. The effective killing of tumor cells was achieved by low effector/target ratios ranging from 0.5:1 to 4:1. CLM provides highly sensitive, safe,more » and fast procedure for measurement of NK cell activity with small blood samples such as those obtained from pediatric patients.« less

Development of a SIDA-LC-MS/MS Method for the Determination of Phomopsin A in Legumes.

PubMed

Schloß, Svenja; Koch, Matthias; Rohn, Sascha; Maul, Ronald

2015-12-09

A novel method for the determination of phomopsin A (1) in lupin flour, pea flour, and bean flour as well as whole lupin plants was established based on stable isotope dilution assay (SIDA) LC-MS/MS using (15)N6-1 as an isotopically labeled internal standard. Artificially infected samples were used to develop an optimized extraction procedure and sample pretreatment. The limits of detection were 0.5-1 μg/kg for all matrices. The limits of quantitation were 2-4 μg/kg. The method was used to analyze flour samples generated from selected legume seeds and lupin plant samples that had been inoculated with Diaporthe toxica and two further fungal strains. Finally, growing lupin plants infected with D. toxica were investigated to simulate a naturally in-field mycotoxicosis. Toxin levels of up to 10.1 μg/kg of 1 were found in the pods and 7.2 μg/kg in the stems and leaves.

Determination of uranium in tap water by ICP-MS.

PubMed

El Himri, M; Pastor, A; de la Guardia, M

2000-05-01

A fast and accurate procedure has been developed for the determination of uranium at microg L(-1) level in tap and mineral water. The method is based on the direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma mass spectrometer (ICP-MS). Uranium was determined at the mass number 238 using Rh as internal standard. The method provides a limit of detection of 2 ng L(-1) and a good repeatability with relative standard deviation values (RSD) about 3% for five independent analyses of samples containing 73 microg L(-1) of uranium. Recovery percentage values found for the determination of uranium in spiked natural samples varied between 91% and 106%. Results obtained are comparable with those found by radiochemical methods for natural samples and of the same order for the certified content of a reference material, thus indicating the accuracy of the ICP-MS procedure without the need of using isotope dilution. A series of mineral and tap waters from different parts of Spain and Morocco were analysed.

Effects of Moisture and Particle Size on Quantitative Determination of Total Organic Carbon (TOC) in Soils Using Near-Infrared Spectroscopy.

PubMed

Tamburini, Elena; Vincenzi, Fabio; Costa, Stefania; Mantovi, Paolo; Pedrini, Paola; Castaldelli, Giuseppe

2017-10-17

Near-Infrared Spectroscopy is a cost-effective and environmentally friendly technique that could represent an alternative to conventional soil analysis methods, including total organic carbon (TOC). Soil fertility and quality are usually measured by traditional methods that involve the use of hazardous and strong chemicals. The effects of physical soil characteristics, such as moisture content and particle size, on spectral signals could be of great interest in order to understand and optimize prediction capability and set up a robust and reliable calibration model, with the future perspective of being applied in the field. Spectra of 46 soil samples were collected. Soil samples were divided into three data sets: unprocessed, only dried and dried, ground and sieved, in order to evaluate the effects of moisture and particle size on spectral signals. Both separate and combined normalization methods including standard normal variate (SNV), multiplicative scatter correction (MSC) and normalization by closure (NCL), as well as smoothing using first and second derivatives (DV1 and DV2), were applied to a total of seven cases. Pretreatments for model optimization were designed and compared for each data set. The best combination of pretreatments was achieved by applying SNV and DV2 on partial least squares (PLS) modelling. There were no significant differences between the predictions using the three different data sets ( p < 0.05). Finally, a unique database including all three data sets was built to include all the sources of sample variability that were tested and used for final prediction. External validation of TOC was carried out on 16 unknown soil samples to evaluate the predictive ability of the final combined calibration model. Hence, we demonstrate that sample preprocessing has minor influence on the quality of near infrared spectroscopy (NIR) predictions, laying the ground for a direct and fast in situ application of the method. Data can be acquired outside the laboratory since the method is simple and does not need more than a simple band ratio of the spectra.

Surface-enhanced Raman spectroscopy studies of yellow organic dyestuffs and lake pigments in oil paint.

PubMed

Mayhew, Hannah E; Fabian, David M; Svoboda, Shelley A; Wustholz, Kristin L

2013-08-21

Identifying natural, organic dyes and pigments is important for the conservation, preservation, and historical interpretation of works of art. Although previous SERS studies have demonstrated high sensitivity and selectivity for red lake pigments using various pretreatment conditions, corresponding investigations of yellow lake pigments and paints are relatively sparse. Here, surface-enhanced Raman scattering (SERS) spectroscopy is used to identify a variety of yellow organic dyestuffs and lake pigments in oil paint. High-quality SERS spectra of yellow dyestuffs (i.e., turmeric, old fustic, Buckthorn berries) and corresponding paints could be obtained with or without sample pretreatment using microliter quantities of HCl and methanol at room temperature. However, the SERS spectra of yellow lake pigments (i.e., Stil de Grain, Reseda lake) and their corresponding oil paints were only observed upon sample pretreatment. Ultimately, we demonstrate a reliable sample treatment protocol for SERS-based identification of turmeric, old fustic, Buckthorn berries, Stil de Grain, and Reseda lake as well as for microscopic samples of the corresponding oil paints.

Meso level multi-disciplinary approach for reduction of pre-treatment loss to follow-up in Revised National Tuberculosis Control Program, Delhi, India.

PubMed

Sharma, Nandini; Chandra, Shivani; Dhuria, Meera; Kohli, Charu; Chopra, Kamal Kishore; Aggarwal, Nishi; Sachdeva, Kuldeep

2017-10-01

Universal access to tuberculosis (TB) care services emphasizes early detection and initiation of treatment for all pulmonary TB patients. Pre-treatment loss to follow-up patients needs to be actively tracked and treated to break the chain of transmission in the community. MATERIALS AND METHODS: A questionnaire based cross sectional study of a sample of 340 patients who were pre-treatment loss to follow-up was conducted from November 2011 to March 2012 in Delhi. Qualitative study involved focused group discussions with paramedical providers using a topic outline guide, patients were interviewed using semi-structured questionnaire and brainstorming of program managers to elicit reasons, suggestions and health seeking behavior among those who were pre-treatment loss to follow-up. Preference for private practitioners (64.4%), lack of trust in government health system (26.7%), inconvenient time of Directly Observed Treatment (DOT) centre (18.5%) and wrong patient address (14%) were the main reasons for pre-treatment loss to follow-up. Paramedical provider's opinion elicited in focused group discussion was that there is an increased tendency of pre-treatment loss to follow-up in drug addicts and home-less patients. Brainstorming with program managers revealed that a lack of trust in allopathic system of medicine and human resource constraints were the leading causes of pre-treatment loss to follow-up. A Meso level multi disciplinary model with community participation through Resident Welfare Associations (RWAs) has been designed based on the above findings. The model suggests mutual collaboration between government and non government agencies for promotion of International Standards of TB care in private clinics, de addiction services and social welfare schemes through RWAs. There is a need for Advocacy Communication and Social Mobilization on a large scale. Collaboration with Resident Welfare Associations (RWAs) and with practitioners from alternate systems of medicine should be encouraged. Copyright © 2017 Tuberculosis Association of India. Published by Elsevier B.V. All rights reserved.

Impact of cultivar selection and process optimization on ethanol yield from different varieties of sugarcane

PubMed Central

2014-01-01

Background The development of ‘energycane’ varieties of sugarcane is underway, targeting the use of both sugar juice and bagasse for ethanol production. The current study evaluated a selection of such ‘energycane’ cultivars for the combined ethanol yields from juice and bagasse, by optimization of dilute acid pretreatment optimization of bagasse for sugar yields. Method A central composite design under response surface methodology was used to investigate the effects of dilute acid pretreatment parameters followed by enzymatic hydrolysis on the combined sugar yield of bagasse samples. The pressed slurry generated from optimum pretreatment conditions (maximum combined sugar yield) was used as the substrate during batch and fed-batch simultaneous saccharification and fermentation (SSF) processes at different solid loadings and enzyme dosages, aiming to reach an ethanol concentration of at least 40 g/L. Results Significant variations were observed in sugar yields (xylose, glucose and combined sugar yield) from pretreatment-hydrolysis of bagasse from different cultivars of sugarcane. Up to 33% difference in combined sugar yield between best performing varieties and industrial bagasse was observed at optimal pretreatment-hydrolysis conditions. Significant improvement in overall ethanol yield after SSF of the pretreated bagasse was also observed from the best performing varieties (84.5 to 85.6%) compared to industrial bagasse (74.5%). The ethanol concentration showed inverse correlation with lignin content and the ratio of xylose to arabinose, but it showed positive correlation with glucose yield from pretreatment-hydrolysis. The overall assessment of the cultivars showed greater improvement in the final ethanol concentration (26.9 to 33.9%) and combined ethanol yields per hectare (83 to 94%) for the best performing varieties with respect to industrial sugarcane. Conclusions These results suggest that the selection of sugarcane variety to optimize ethanol production from bagasse can be achieved without adversely affecting juice ethanol and cane yield, thus maintaining first generation ethanol production levels while maximizing second generation ethanol production. PMID:24725458

Effect of microwave hydrolysis on transformation of steroidal hormones during anaerobic digestion of municipal sludge cake.

PubMed

Hamid, Hanna; Eskicioglu, Cigdem

2013-09-15

Fate and removal of 16 steroidal (estrogenic, androgenic and progestogenic) hormones were studied during advanced anaerobic digestion of sludge cake using microwave (MW) pretreatment. Effect of pretreatment temperature (80, 120, 160 °C), operating temperature (mesophilic at 35 ± 2 °C, thermophilic at 55 ± 2 °C) and sludge retention time (SRT: 20, 10, 5 days) were studied employing eight lab-scale semi-continuously fed digesters. To determine the potential effect of MW hydrolysis, hormones were quantified in total (sorbed + soluble) and supernatant (soluble) phases of the digester influent and effluent streams. Seven of 16 hormones were above the method reporting limit (RL) in one or more of the samples. Hormone concentrations in total phase of un-pretreated (control) and pretreated digester feeds ranged in <157-2491 ng/L and <157-749 ng/L, respectively. The three studied factors were found to be statistically significant (95% confidence level) in removal of one or more hormones from soluble and/or total phase. MW hydrolysis of the influent resulted in both release (from sludge matrix) and attenuation of hormones in the soluble phase. Accumulation of estrone (E1) as well as progesterone (Pr) and androstenedione (Ad) in most of the digesters indicated possible microbial transformations among the hormones. Compared to controls, all pretreated digesters had lower total hormone concentrations in their influent streams. At 20 days SRT, highest total removal (E1+E2+Ad +Pr) was observed for the thermophilic control digester (56%), followed by pretreated mesophilic digesters at 120 °C and 160 °C with around 48% efficiency. In terms of conventional performance parameters, relative (to control) improvements of MW pretreated digesters at a 5-d SRT ranged in 98-163% and 57-121%, for volatile solids removal and methane production, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Production of high concentrated cellulosic ethanol by acetone/water oxidized pretreated beech wood.

PubMed

Katsimpouras, Constantinos; Kalogiannis, Konstantinos G; Kalogianni, Aggeliki; Lappas, Angelos A; Topakas, Evangelos

2017-01-01

Lignocellulosic biomass is an abundant and inexpensive resource for biofuel production. Alongside its biotechnological conversion, pretreatment is essential to enable efficient enzymatic hydrolysis by making cellulose susceptible to cellulases. Wet oxidation of biomass, such as acetone/water oxidation, that employs hot acetone, water, and oxygen, has been found to be an attractive pretreatment method for removing lignin while producing less degradation products. The remaining enriched cellulose fraction has the potential to be utilized under high gravity enzymatic saccharification and fermentation processes for the cost-competing production of bioethanol. Beech wood residual biomass was pretreated following an acetone/water oxidation process aiming at the production of high concentration of cellulosic ethanol. The effect of pressure, reaction time, temperature, and acetone-to-water ratio on the final composition of the pretreated samples was studied for the efficient utilization of the lignocellulosic feedstock. The optimal conditions were acetone/water ratio 1:1, 40 atm initial pressure of 40 vol% O 2 gas, and 64 atm at reaction temperature of 175 °C for 2 h incubation. The pretreated beech wood underwent an optimization step studying the effect of enzyme loading and solids content on the enzymatic liquefaction/saccharification prior to fermentation. In a custom designed free-fall mixer at 50 °C for either 6 or 12 h of prehydrolysis using an enzyme loading of 9 mg/g dry matter at 20 wt% initial solids content, high ethanol concentration of 75.9 g/L was obtained. The optimization of the pretreatment process allowed the efficient utilization of beech wood residual biomass for the production of high concentrations of cellulosic ethanol, while obtaining lignin that can be upgraded towards high-added-value chemicals. The threshold of 4 wt% ethanol concentration that is required for the sustainable bioethanol production was surpassed almost twofold, underpinning the efficient conversion of biomass to ethanol and bio-based chemicals on behalf of the biorefinery concept.

Development of a system for characterizing biomass quality of lignocellulosic feedstocks for biochemical conversion

NASA Astrophysics Data System (ADS)

Murphy, Patrick Thomas

The purpose of this research was twofold: (i) to develop a system for screening lignocellulosic biomass feedstocks for biochemical conversion to biofuels and (ii) to evaluate brown midrib corn stover as feedstock for ethanol production. In the first study (Chapter 2), we investigated the potential of corn stover from bm1-4 hybrids for increased ethanol production and reduced pretreatment intensity compared to corn stover from the isogenic normal hybrid. Corn stover from hybrid W64A X A619 and respective isogenic bm hybrids was pretreated by aqueous ammonia steeping using ammonium hydroxide concentrations from 0 to 30%, by weight, and the resulting residues underwent simultaneous saccharification and cofermentation (SSCF) to ethanol. Dry matter (DM) digested by SSCF increased with increasing ammonium hydroxide concentration across all genotypes (P>0.0001) from 277 g kg-1 DM in the control to 439 g kg-1 DM in the 30% ammonium hydroxide pretreatment. The bm corn stover materials averaged 373 g kg-1 DM of DM digested by SSCF compared with 335 g kg-1 DM for the normal corn stover (P<0.0001). Of the bm mutations, bm3 had (i) the greatest effect on cell-wall carbohydrate hydrolysis of corn stover, (ii) the lowest initial cell-wall carbohydrate concentration, (iii) the lowest dry matter remaining after pretreatment, and (iv) the highest amount of monosaccharides released during enzymatic hydrolysis. However, bm corn stover did not reduce the severity of aqueous ammonia steeping pretreatment needed to maximize DM hydrolysis during SSCF compared with normal corn stover. In the remaining studies (Chapters 3 thru 5), a system for analyzing the quality of lignocellulosic biomass feedstocks for biochemical conversion to biofuels (i.e., pretreatment, enzymatic hydrolysis, and fermentation) was developed. To accomplish this, a carbohydrate availability model was developed to characterize feedstock quality. The model partitions carbohydrates within a feedstock material into fractions based on their availability to be converted to fermentable sugars, including non-structural carbohydrates (CN) (monosaccharides, starches, oligosaccharides), biochemically available carbohydrates (CB) (structural carbohydrates susceptible to enzymatic hydrolysis) with an associated 1st-order availability rate constant (k B) and unavailable carbohydrates (CU) (hemicellulose and cellulose in close association with lignin). The model partitions the noncarbohydrate dry matter into extractives, lignin, and ash. Quality parameters were determined using a biomass quality assay that combined established wet-chemistry analyses techniques, including total non-structural carbohydrates (TNC), alcohol insoluble residue (AIR), simultaneous saccharification and fermentation (SSCF), and Klason lignin. The next study evaluated multiple high-throughput (HTP) modifications to the original assay methods, including (i) using filter bags with batch sample processing, (ii) replacement of AIR with neutral detergent fiber (NDF) as a cell-wall isolation procedure, and (iii) elimination of the fermentation organism in the SSCF procedures used to determine biochemically available carbohydrates. The original and the HTP assay methods were compared using corn cobs, hybrid poplar, kenaf, and switchgrass. Biochemically available carbohydrates increased with the HTP methods in the corn cobs, hybrid poplar, and switchgrass, but remained the same in the kenaf. Total available carbohydrates increased and unavailable carbohydrates decreased with the HTP methods in the corn cobs and switchgrass and remained the same in the hybrid poplar and kenaf. There were no differences in total carbohydrates (CT) between the two methods. The final study evaluated the variability of biomass quality parameters in a set of corn stover samples, and developed calibration equations for determining parameter values using near infrared reflectance spectroscopy (NIRS). Fifty-two corn stover samples harvested in Iowa and Wisconsin in 2005 and 2006 were analyzed using the HTP assay for determining feedstock quality for biochemical conversion. Non-structural carbohydrates ranged from 84 to 155 g kg -1 DM, CB ranged from 354 to 557 g kg-1 DM, kB ranged from 0.20 to 0.33 h-1, CA ranged from 463 to 699 g kg-1 DM, and neutral detergent lignin (NDL) ranged from 32 to 74 g kg-1 DM. Significant differences (P<0.0001) among samples were observed for all parameters, except for the availability rate constant of CB. (Abstract shortened by UMI.)

Piezoelectric immunochip for the detection of dengue fever in viremia phase.

PubMed

Wu, Tzong-Zeng; Su, Chih-Cheng; Chen, Li-Kuang; Yang, Hui-Hua; Tai, Dar-Fu; Peng, Kou-Cheng

2005-11-15

The global prevalence of dengue fever has grown so dramatically in recent years that it is endemic in more than 100 countries and has become a major international public health concern. Moreover, since the flu-like symptoms that accompany dengue fever are atypical and varied, the detection procedures currently used to identify it are cumbersome and time-consuming, making early stage epidemiological control and effective medical treatment of this epidemic almost impossible. In this study, a QCM-based detection system was developed in which two monoclonal antibodies against dengue E and NS-1 protein, respectively, were control orientated immobilized on QCM via protein A to produce an immunochip. Various sample pretreatment procedures were evaluated to ascertain the most suitable combination, and both the simulating samples and the clinical specimen were examined by the immunochip. The results revealed that the cibacron blue 3GA gel-heat denature (CB-HD) method was the most effective sample pretreatment technique. Due to the complex composition of the serum, the immunochip could only effectively quantify dengue viral antigens in a 1/1000 untreated simulated sample. With the help of the CB-HD method, the dilution folds were found to capable of being reduced from 1000 to 100, and the detection limit lowered to 1.727 microg/ml (E protein) and 0.740 microg/ml (NS-1 protein) in the original sample. While the cocktail immunochip could not quantify both antigens separately, the higher signal level rendered it a more effective qualification tool for suspect screening. Moreover, the results of the analysis of clinical specimens also proved the ability and future potential of cocktail immunochip in discriminating dengue-positive cases from negative serum specimens in the viremia phase.

Analytical Approaches to Understanding the Role of Non-carbohydrate Components in Wood Biorefinery

NASA Astrophysics Data System (ADS)

Leskinen, Timo Ensio

This dissertation describes the production and analysis of wood subjected to a novel electron beam-steam explosion pretreatment (EB-SE) pretreatment with the aim to evaluate its suitability for the production of bioethanol. The goal of these studies was to: 1) develop analytical methods for the investigation of depolymerization of wood components under pretreatments, 2) analyze the effects of EB-SE pretreatment on the pretreated biomass, 3) define how lignin and extractive components affect the action of enzymes on cellulosic substrates, and 4) examine how changes in lignin structure impact its isolation and potential conversion into value added chemicals. The first section of the work describes the development of a size-exclusion chromatography (SEC) methodology for molecular weight analysis for native and pretreated wood. The selective analysis of carbohydrates and lignin from native wood was made possible by the combination of two selective derivatization methods, ionic liquid assisted benzoylation of the carbohydrate fraction and acetobromination of the lignin in acetic acid media. This method was then used to examine changes in softwood samples after the EB-SE pretreatment. The methodology was shown to be effective for monitoring changes in the molecular weight profiles of the pretreated wood. The second section of the work investigates synergistic effects of the EB-SE pretreatment on the molecular level structures of wood components and the significance of these alterations in terms of enzymatic digestibility. The two pretreatment steps depolymerized cell wall components in different fashion, while showing synergistic effects. Hardwood and softwood species responded differently to similar treatment conditions, which was attributed to the well-known differences in the structure of their lignin and hemicellulose fractions. The relatively crosslinked lignin in softwood appeared to limit swelling and subsequent depolymerization in comparison to hardwood. Additional studies revealed that an insoluble, likely crosslinked, lignin fraction induced enzyme inhibition, while soluble lower molecular weight fractions were slightly beneficial for the enzymatic hydrolysis of cellulose. The third section of the work addresses the influence of hydrophobic wood extractives and representative model compounds on the cellulolytic hydrolysis of cellulosic substrates. Deposition of specific fractions of isolated wood extractives on cellulose was found either to enhance or inhibit the action of cellulase enzymes, depending on the chemical nature of the fraction. Using model compounds this effect was found to be correlated with the compounds chemical structure, and underlying mechanisms could be rationalized by Hansen solubility parameter considerations. The amphiphilic and hydrophobic nature of the model extractives was found to influence the deposition of extractives on the cellulose surfaces, and the adsorption of cellulolytic enzymes, as measured with Quartz Crystal Microgravimetry. Beneficial effects of the extractives were likely related to reduction in the irreversible binding of the enzymes on the cellulose substrate. The fourth section of the work deals with the recovery of lignin using extraction methods based on aqueous alkali or aqueous ethanol. The objective of this study was to understand how the yield, MW and structure of lignin recovered from the process residue was impacted by the different isolation methods. Mild extraction conditions allowed for recovery of approximately 40 wt.% of the lignin present in the process residues. Base or acid catalyzed hydrolysis of the lignin could increase the recovery lignin yield to about 76 wt.%. The recovered lignins were characterized in terms of their functional groups, molecular weights and thermal properties. The lignins from mild alkali and ethanol extractions showed similarities in their chemical profiles while, as expected, the hydrolyzed lignins were different and depended on the hydrolysis conditions. The molecular weight and thermal properties of the lignin products were affected by the applied isolation process.

[Determination of eight pesticide residues in tea by liquid chromatography-tandem mass spectrometry and its uncertainty evaluation].

PubMed

Hu, Beizhen; Cai, Haijiang; Song, Weihua

2012-09-01

A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C, column (150 mm x 2. 1 mm, 5 microm) and with the gradient elution of acetonitrile and 0. 1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 - 100 microg/L for fipronil, and in 5 -200 microg/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 p.g/kg for fipronil and 10 microg/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115.0% with the relative standard deviations of 2.7% - 7.7% at the spiked levels of 2, 5, 50 microg/kg for fipronil and 10, 50, 100 microg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea.

Gradient elution moving boundary electrophoresis enables rapid analysis of acids in complex biomass-derived streams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Munson, Matthew S.; Karp, Eric M.; Nimlos, Claire T.

Biomass conversion processes such as pretreatment, liquefaction, and pyrolysis often produce complex mixtures of intermediates that are a substantial challenge to analyze rapidly and reliably. To characterize these streams more comprehensively and efficiently, new techniques are needed to track species through biomass deconstruction and conversion processes. Here, we present the application of an emerging analytical method, gradient elution moving boundary electrophoresis (GEMBE), to quantify a suite of acids in a complex, biomass-derived streams from alkaline pretreatment of corn stover. GEMBE offers distinct advantages over common chromatography-spectrometry analytical approaches in terms of analysis time, sample preparation requirements, and cost of equipment.more » As demonstrated here, GEMBE is able to track 17 distinct compounds (oxalate, formate, succinate, malate, acetate, glycolate, protocatechuate, 3-hydroxypropanoate, lactate, glycerate, 2-hydroxybutanoate, 4-hydroxybenzoate, vanillate, p-coumarate, ferulate, sinapate, and acetovanillone). The lower limit of detection was compound dependent and ranged between 0.9 and 3.5 umol/L. Results from GEMBE were similar to recent results from an orthogonal method based on GCxGC-TOF/MS. Altogether, GEMBE offers a rapid, robust approach to analyze complex biomass-derived samples, and given the ease and convenience of deployment, may offer an analytical solution for online tracking of multiple types of biomass streams.« less

Gradient elution moving boundary electrophoresis enables rapid analysis of acids in complex biomass-derived streams

DOE PAGES

Munson, Matthew S.; Karp, Eric M.; Nimlos, Claire T.; ...

2016-09-27

Biomass conversion processes such as pretreatment, liquefaction, and pyrolysis often produce complex mixtures of intermediates that are a substantial challenge to analyze rapidly and reliably. To characterize these streams more comprehensively and efficiently, new techniques are needed to track species through biomass deconstruction and conversion processes. Here, we present the application of an emerging analytical method, gradient elution moving boundary electrophoresis (GEMBE), to quantify a suite of acids in a complex, biomass-derived streams from alkaline pretreatment of corn stover. GEMBE offers distinct advantages over common chromatography-spectrometry analytical approaches in terms of analysis time, sample preparation requirements, and cost of equipment.more » As demonstrated here, GEMBE is able to track 17 distinct compounds (oxalate, formate, succinate, malate, acetate, glycolate, protocatechuate, 3-hydroxypropanoate, lactate, glycerate, 2-hydroxybutanoate, 4-hydroxybenzoate, vanillate, p-coumarate, ferulate, sinapate, and acetovanillone). The lower limit of detection was compound dependent and ranged between 0.9 and 3.5 umol/L. Results from GEMBE were similar to recent results from an orthogonal method based on GCxGC-TOF/MS. Altogether, GEMBE offers a rapid, robust approach to analyze complex biomass-derived samples, and given the ease and convenience of deployment, may offer an analytical solution for online tracking of multiple types of biomass streams.« less

Soil pretreatment and fast cell lysis for direct polymerase chain reaction from forest soils for terminal restriction fragment length polymorphism analysis of fungal communities

Treesearch

Fei Cheng; Lin Hou; Keith Woeste; Zhengchun Shang; Xiaobang Peng; Peng Zhao; Shuoxin Zhang

2016-01-01

Humic substances in soil DNA samples can influence the assessment of microbial diversity and community composition. Using multiple steps during or after cell lysis adds expenses, is time-consuming, and causes DNA loss. A pretreatment of soil samples and a single step DNA extraction may improve experimental results. In order to optimize a protocol for obtaining high...

Insights on the Effects of Heat Pretreatment, pH, and Calcium Salts on Isolation of Rare Actinobacteria from Karstic Caves

PubMed Central

Fang, Bao-Zhu; Salam, Nimaichand; Han, Ming-Xian; Jiao, Jian-Yu; Cheng, Juan; Wei, Da-Qiao; Xiao, Min; Li, Wen-Jun

2017-01-01

The phylum Actinobacteria is one of the most ubiquitously present bacterial lineages on Earth. In the present study, we try to explore the diversity of cultivable rare Actinobacteria in Sigangli Cave, Yunnan, China by utilizing a combination of different sample pretreatments and under different culture conditions. Pretreating the samples under different conditions of heat, setting the isolation condition at different pHs, and supplementation of media with different calcium salts were found to be effective for isolation of diverse rare Actinobacteria. During our study, a total of 204 isolates affiliated to 30 genera of phylum Actinobacteria were cultured. Besides the dominant Streptomyces, rare Actinobacteria of the genera Actinocorallia, Actinomadura, Agromyces, Alloactinosynnema, Amycolatopsis, Beutenbergia, Cellulosimicrobium, Gordonia, Isoptericola, Jiangella, Knoellia, Kocuria, Krasilnikoviella, Kribbella, Microbacterium, Micromonospora, Mumia, Mycobacterium, Nocardia, Nocardioides, Nocardiopsis, Nonomuraea, Oerskovia, Pseudokineococcus, Pseudonocardia, Rhodococcus, Saccharothrix, Streptosporangium, and Tsukamurella were isolated from these cave samples. PMID:28848538

Improvement of near infrared spectroscopic (NIRS) analysis of caffeine in roasted Arabica coffee by variable selection method of stability competitive adaptive reweighted sampling (SCARS).

PubMed

Zhang, Xuan; Li, Wei; Yin, Bin; Chen, Weizhong; Kelly, Declan P; Wang, Xiaoxin; Zheng, Kaiyi; Du, Yiping

2013-10-01

Coffee is the most heavily consumed beverage in the world after water, for which quality is a key consideration in commercial trade. Therefore, caffeine content which has a significant effect on the final quality of the coffee products requires to be determined fast and reliably by new analytical techniques. The main purpose of this work was to establish a powerful and practical analytical method based on near infrared spectroscopy (NIRS) and chemometrics for quantitative determination of caffeine content in roasted Arabica coffees. Ground coffee samples within a wide range of roasted levels were analyzed by NIR, meanwhile, in which the caffeine contents were quantitative determined by the most commonly used HPLC-UV method as the reference values. Then calibration models based on chemometric analyses of the NIR spectral data and reference concentrations of coffee samples were developed. Partial least squares (PLS) regression was used to construct the models. Furthermore, diverse spectra pretreatment and variable selection techniques were applied in order to obtain robust and reliable reduced-spectrum regression models. Comparing the respective quality of the different models constructed, the application of second derivative pretreatment and stability competitive adaptive reweighted sampling (SCARS) variable selection provided a notably improved regression model, with root mean square error of cross validation (RMSECV) of 0.375 mg/g and correlation coefficient (R) of 0.918 at PLS factor of 7. An independent test set was used to assess the model, with the root mean square error of prediction (RMSEP) of 0.378 mg/g, mean relative error of 1.976% and mean relative standard deviation (RSD) of 1.707%. Thus, the results provided by the high-quality calibration model revealed the feasibility of NIR spectroscopy for at-line application to predict the caffeine content of unknown roasted coffee samples, thanks to the short analysis time of a few seconds and non-destructive advantages of NIRS. Copyright © 2013 Elsevier B.V. All rights reserved.

Improvement of near infrared spectroscopic (NIRS) analysis of caffeine in roasted Arabica coffee by variable selection method of stability competitive adaptive reweighted sampling (SCARS)

NASA Astrophysics Data System (ADS)

Zhang, Xuan; Li, Wei; Yin, Bin; Chen, Weizhong; Kelly, Declan P.; Wang, Xiaoxin; Zheng, Kaiyi; Du, Yiping

2013-10-01

Coffee is the most heavily consumed beverage in the world after water, for which quality is a key consideration in commercial trade. Therefore, caffeine content which has a significant effect on the final quality of the coffee products requires to be determined fast and reliably by new analytical techniques. The main purpose of this work was to establish a powerful and practical analytical method based on near infrared spectroscopy (NIRS) and chemometrics for quantitative determination of caffeine content in roasted Arabica coffees. Ground coffee samples within a wide range of roasted levels were analyzed by NIR, meanwhile, in which the caffeine contents were quantitative determined by the most commonly used HPLC-UV method as the reference values. Then calibration models based on chemometric analyses of the NIR spectral data and reference concentrations of coffee samples were developed. Partial least squares (PLS) regression was used to construct the models. Furthermore, diverse spectra pretreatment and variable selection techniques were applied in order to obtain robust and reliable reduced-spectrum regression models. Comparing the respective quality of the different models constructed, the application of second derivative pretreatment and stability competitive adaptive reweighted sampling (SCARS) variable selection provided a notably improved regression model, with root mean square error of cross validation (RMSECV) of 0.375 mg/g and correlation coefficient (R) of 0.918 at PLS factor of 7. An independent test set was used to assess the model, with the root mean square error of prediction (RMSEP) of 0.378 mg/g, mean relative error of 1.976% and mean relative standard deviation (RSD) of 1.707%. Thus, the results provided by the high-quality calibration model revealed the feasibility of NIR spectroscopy for at-line application to predict the caffeine content of unknown roasted coffee samples, thanks to the short analysis time of a few seconds and non-destructive advantages of NIRS.

Determination of residual solvents in pharmaceuticals by thermal desorption-GC/MS.

PubMed

Hashimoto, K; Urakami, K; Fujiwara, Y; Terada, S; Watanabe, C

2001-05-01

A novel method for the determination of residual solvents in pharmaceuticals by thermal desorption (TD)-GC/MS has been established. A programmed temperature pyrolyzer (double shot pyrolyzer) is applied for the TD. This method does not require any sample pretreatment and allows very small amounts of the sample. Directly desorbed solvents from intact pharmaceuticals (ca. 1 mg) in the desorption cup (5 mm x 3.8 mm i.d.) were cryofocused at the head of a capillary column prior to a GC/MS analysis. The desorption temperature was set at a point about 20 degrees C higher than the melting point of each sample individually, and held for 3 min. The analytical results using 7 different pharmaceuticals were in agreement with those obtained by direct injection (DI) of the solution, followed by USP XXIII. This proposed TD-GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents. Furthermore, this method was simple, allowed rapid analysis and gave good repeatability.

Simultaneous Determination of Isopyrazam and Azoxystrobin in Cucumbers by Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Hu, Dan; Xu, Xu; Cai, Tian; Wang, Wei-Ying; Wu, Chun-Jie; Ye, Li-Ming

2017-12-01

A rapid and sensitive analytical method based on high-performance liquid chromatography-tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg -1 (n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg -1 , respectively, which are far below the maximum residue level (0.5 mg kg -1 ) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.

A rapid and sensitive LC-MS/MS method for the determination of Pulsatilla saponin D in rat plasma and its application in a rat pharmacokinetic and bioavailability study.

PubMed

Ouyang, Hui; Guo, Yicheng; He, Mingzhen; Zhang, Jinlian; Huang, Xiaofang; Zhou, Xin; Jiang, Hongliang; Feng, Yulin; Yang, Shilin

2015-03-01

A simple, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of Pulsatilla saponin D, a potential antitumor constituent isolated from Pulsatilla chinensis in rat plasma. Rat plasma samples were pretreated by protein precipitation with methanol. The method validation was performed in accordance with US Food and Drug Administration guidelines and the results met the acceptance criteria. The method was successfully applied to assess the pharmacokinetics and oral bioavailability of Pulsatilla saponin D in rats. Copyright © 2014 John Wiley & Sons, Ltd.

Extended Performance Assessment in Accelerated Corrosion and Adhesion of CARC Prepared Aluminum Alloy 5059-H131 for Three Different Pretreatment Methods

DTIC Science & Technology

2008-03-01

conversion coating, only works well as part of a complete coating system as was the case in this study. Trivalent chromium pretreatments such as TCP must...conditions. The pretreatment conditions were abrasive blasted, a nonchromate pretreatment (NCP)1, and a commercial trivalent chromate pretreatment...ease of manufacturing via welds , excellent performance against fragmentation based threats, and excellent corrosion resistance. As threat levels have

[Discrimination of varieties of brake fluid using visual-near infrared spectra].

PubMed

Jiang, Lu-lu; Tan, Li-hong; Qiu, Zheng-jun; Lu, Jiang-feng; He, Yong

2008-06-01

A new method was developed to fast discriminate brands of brake fluid by means of visual-near infrared spectroscopy. Five different brands of brake fluid were analyzed using a handheld near infrared spectrograph, manufactured by ASD Company, and 60 samples were gotten from each brand of brake fluid. The samples data were pretreated using average smoothing and standard normal variable method, and then analyzed using principal component analysis (PCA). A 2-dimensional plot was drawn based on the first and the second principal components, and the plot indicated that the clustering characteristic of different brake fluid is distinct. The foregoing 6 principal components were taken as input variable, and the band of brake fluid as output variable to build the discriminate model by stepwise discriminant analysis method. Two hundred twenty five samples selected randomly were used to create the model, and the rest 75 samples to verify the model. The result showed that the distinguishing rate was 94.67%, indicating that the method proposed in this paper has good performance in classification and discrimination. It provides a new way to fast discriminate different brands of brake fluid.

Pretreatment with low-energy shock waves reduces the renal oxidative stress and inflammation caused by high-energy shock wave lithotripsy.

PubMed

Clark, Daniel L; Connors, Bret A; Handa, Rajash K; Evan, Andrew P

2011-12-01

The purpose of this study was to determine if pretreatment of porcine kidneys with low-energy shock waves (SWs) prior to delivery of a clinical dose of 2,000 SWs reduces or prevents shock wave lithotripsy (SWL)-induced acute oxidative stress and inflammation in the treated kidney. Pigs (7-8 weeks old) received 2,000 SWs at 24 kV (120 SW/min) with or without pretreatment with 100 SWs at 12 kV/2 Hz to the lower pole calyx of one kidney using the HM3. Four hours post-treatment, selected samples of renal tissue were frozen for analysis of cytokine, interleukin-6 (IL-6), and stress response protein, heme oxygenase-1 (HO-1). Urine samples were taken before and after treatment for analysis of tumor necrosis factor-α (TNF-α). Treatment with 2,000 SWs with or without pretreatment caused a statistically significant elevation of HO-1 and IL-6 in the renal medulla localized to the focal zone of the lithotripter. However, the increase in HO-1 and IL-6 was significantly reduced using the pretreatment protocol compared to no pretreatment. Urinary excretion of TNF-α increased significantly (p < 0.05) from baseline for pigs receiving 2,000 SWs alone; however, this effect was completely abolished with the pretreatment protocol. We conclude that pretreatment of the kidney with a low dose of low-energy SWs prior to delivery of a clinical dose of SWs reduces, but does not completely prevent, SWL-induced acute renal oxidative stress and inflammation.

Low melting point pyridinium ionic liquid pretreatment for enhancing enzymatic saccharification of cellulosic biomass.

PubMed

Uju; Nakamoto, Aya; Shoda, Yasuhiro; Goto, Masahiro; Tokuhara, Wataru; Noritake, Yoshiyuki; Katahira, Satoshi; Ishida, Nobuhiro; Ogino, Chiaki; Kamiya, Noriho

2013-05-01

The potential of 1-hexylpyridinium chloride ([Hpy][Cl]), to pretreat cellulosic feedstocks was investigated using microcrystalline cellulose (Avicel) and Bagasse at 80 °C or 100 °C. Short [Hpy][Cl] pretreatments, <30 min, at lower temperature accelerate subsequent enzymatic saccharification of Avicel. Over 95% conversion of pretreated Avicel to glucose was attained after 24h enzymatic saccharification under optimal conditions, whereas regenerated Bagasse showed 1-3-fold higher conversion than untreated biomass. FT-IR analysis of both Avicel and Bagasse samples pretreated with [Hpy][Cl] or 1-ethyl-3-methyimidazolium acetate ([Emim][OAc]) revealed that these ionic liquids behaved differently during pretreatment. [Hpy][Cl] pretreatment for an extended duration (180 min) released mono- and disaccharides without using cellulase enzymes, suggesting [Hpy][Cl] has capability for direct saccharification of cellulosic feedstocks. On the basis of the results obtained, [Hpy][Cl] pretreatment enhanced initial reaction rates in enzymatic saccharification by either crystalline polymorphic alteration of cellulose or partial degradation of the crystalline cellulosic fraction in biomass. Copyright © 2012 Elsevier Ltd. All rights reserved.

Improving the conversion of biomass in catalytic fast pyrolysis via white-rot fungal pretreatment.

PubMed

Yu, Yanqing; Zeng, Yelin; Zuo, Jiane; Ma, Fuying; Yang, Xuewei; Zhang, Xiaoyu; Wang, Yujue

2013-04-01

This study investigated the effect of white-rot fungal pretreatment on corn stover conversion in catalytic fast pyrolysis (CFP). Corn stover pretreated by white-rot fungus Irpex lacteus CD2 was fast pyrolyzed alone (non-CFP) and with ZSM-5 zeolite (CFP) in a semi-batch pyroprobe reactor. The fungal pretreatment considerably increased the volatile product yields (predominantly oxygenated compounds) in non-CFP, indicating that fungal pretreatment enhances the corn stover conversion in fast pyrolysis. In the presence of ZSM-5 zeolite, these oxygenated volatiles were further catalytically converted to aromatic hydrocarbons, whose yield increased from 10.03 wt.% for the untreated corn stover to 11.49 wt.% for the pretreated sample. In contrast, the coke yield decreased from 14.29 to 11.93 wt.% in CFP following the fungal pretreatment. These results indicate that fungal pretreatment can enhance the production of valuable aromatics and decrease the amount of undesired coke, and thus has a beneficial effect on biomass conversion in CFP. Copyright © 2013 Elsevier Ltd. All rights reserved.

Experimental investigation of ionic liquid pretreatment of sugarcane bagasse with 1,3-dimethylimadazolium dimethyl phosphate.

PubMed

Bahrani, Samaneh; Raeissi, Sona; Sarshar, Mohammad

2015-06-01

In this study, an imidazolium-based ionic liquid (IL), 1,3-dimethylimidazolium dimethyl phosphate ([Mmim][DMP]), was applied for pretreating sugarcane bagasse to produce bioethanol. The main goal of this study was to investigate the feasibility of bagasse pretreatment with this IL, and to verify the effect of different operational parameters on the pretreatment process. Results indicated that temperature and duration of IL-pretreatment have optimum values. Within the range investigated, a maximum fermentable sugar conversion of 70.38% was achieved with this IL at 120°C and 120min. The corresponding value was 28.65% for the untreated biomass. The main cause for the observed enhancement in enzymatic hydrolysis was the reduction of cellulose crystallinity in the IL-pretreated biomass, as compared to the untreated sample, because it resulted in higher accessibility of the enzymes to the biomass after pretreatment. Moreover, the results indicated that aqueous [Mmim][DMP] mixtures are not as effective for pretreatment as the pure IL. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of pretreatment on the enzymatic hydrolysis of kitchen waste for xanthan production.

PubMed

Li, Panyu; Zeng, Yu; Xie, Yi; Li, Xiang; Kang, Yan; Wang, Yabo; Xie, Tonghui; Zhang, Yongkui

2017-01-01

The study was carried out to gain insight into the effect of pretreatment on enzymatic hydrolysis of kitchen waste (KW) for xanthan fermentation. Herein, various pretreatments were applied and it was found that chemical pretreatment had positive effect on the following enzymatic or overall hydrolysis process. The highest reducing sugar concentration was obtained as 51.87g/L from 2% HCl (90°C) pretreated sample, while the Kjeldahl nitrogen (KDN) concentration was 7.79g/L. Kinetic study showed that first order kinetic model was suitable to describe the enzymatic hydrolysis process. The obtained kitchen waste hydrolysate (KWH) was successfully applied for xanthan fermentation. Xanthan concentration reached 4.09-6.46g/L when KWH with 2% HCl (90°C) pretreatment was applied as medium. In comparison, a xanthan concentration of 3.25-5.57g/L was obtained from KWH without pretreatment. Therefore, pretreatment of KW using diluted acid is favorable for the overall hydrolysis process and effective for xanthan fermentation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of four pretreatments on enzymatic hydrolysis and ethanol fermentation of wheat straw. Influence of inhibitors and washing.

PubMed

Toquero, Cristina; Bolado, Silvia

2014-04-01

Pretreatment is essential in the production of alcohol from lignocellulosic material. In order to increase enzymatic sugar release and bioethanol production, thermal, dilute acid, dilute basic and alkaline peroxide pretreatments were applied to wheat straw. Compositional changes in pretreated solid fractions and sugars and possible inhibitory compounds released in liquid fractions were analysed. SEM analysis showed structural changes after pretreatments. Enzymatic hydrolysis and fermentation by Pichia stipitis of unwashed and washed samples from each pretreatment were performed so as to compare sugar and ethanol yields. The effect of the main inhibitors found in hydrolysates (formic acid, acetic acid, 5-hydroxymethylfurfural and furfural) was first studied through ethanol fermentations of model media and then compared to real hydrolysates. Hydrolysates of washed alkaline peroxide pretreated biomass provided the highest sugar concentrations, 31.82g/L glucose, and 13.75g/L xylose, their fermentation yielding promising results, with ethanol concentrations reaching 17.37g/L. Copyright © 2014 Elsevier Ltd. All rights reserved.

Associating cooking additives with sodium hydroxide to pretreat bamboo residues for improving the enzymatic saccharification and monosaccharides production.

PubMed

Huang, Caoxing; He, Juan; Wang, Yan; Min, Douyong; Yong, Qiang

2015-10-01

Cooking additive pulping technique is used in kraft mill to increase delignification degree and pulp yield. In this work, cooking additives were firstly applied in the sodium hydroxide pretreatment for improving the bioconversion of bamboo residues to monosaccharides. Meanwhile, steam explosion and sulfuric acid pretreatments were also carried out on the sample to compare their impacts on monosaccharides production. Results indicated that associating anthraquinone with sodium hydroxide pretreatment showed the best performance in improving the original carbohydrates recovery, delignification, enzymatic saccharification, and monosaccharides production. After consecutive pretreatment and enzymatic saccharification process, 347.49 g, 307.48 g, 142.93 g, and 87.15 g of monosaccharides were released from 1000 g dry bamboo residues pretreated by sodium hydroxide associating with anthraquinone, sodium hydroxide, steam explosion and sulfuric acid, respectively. The results suggested that associating cooking additive with sodium hydroxide is an effective pretreatment for bamboo residues to enhance enzymatic saccharification for monosaccharides production. Copyright © 2015 Elsevier Ltd. All rights reserved.

Enhancement of In Situ Enzymatic Saccharification of Corn Stover by a Stepwise Sodium Hydroxide and Organic Acid Pretreatment.

PubMed

Qing, Qing; Guo, Qi; Zhou, Linlin; He, Yucai; Wang, Liqun; Zhang, Yue

2017-01-01

A stepwise pretreatment method that combines sodium hydroxide and organic acid pretreatments was proposed and investigated to maximize the recovery of main constituents of lignocellulose. The sodium hydroxide pretreatment was firstly optimized by a designed orthogonal experiment with the optimum pretreatment conditions determined as 1 wt% NaOH at 70 °C for 1 h, and 60.42 % of lignin was successfully removed during this stage. In the second stage, 0.5 % acetic acid was selected to pretreat the first-stage solid residue at 80 °C for 40 min in order to decompose hemicelluloses to soluble oligomers or monomers. Then, the whole slurry was subjected to in situ enzymatic saccharification by cellullase with a supplementation of xylanase to further degrade the xylooligosaccharides generated during the acetic acid pretreatment. The maximum reducing sugar and glucose yields achieved were 20.74 and 12.03 g/L, respectively. Furthermore, rapid ethanol fermentation and a yield of 80.3 % also testified this pretreatment method, and the in situ saccharification did not bring any negative impact on ethanol fermentation and has a broad application prospect.

Ultrasonic and Thermal Pretreatments on Anaerobic Digestion of Petrochemical Sludge: Dewaterability and Degradation of PAHs

PubMed Central

Zhou, Jun; Xu, Weizhong; Wong, Jonathan W. C.; Yong, Xiaoyu; Yan, Binghua; Zhang, Xueying; Jia, Honghua

2015-01-01

Effects of different pretreatment methods on sludge dewaterability and polycyclic aromatic hydrocarbons (PAHs) degradation during petrochemical sludge anaerobic digestion were studied. Results showed that the total biogas production volume in the thermal pretreatment system was 4 and 5 times higher than that in the ultrasound pretreatment and in the control system, and the corresponding volatile solid removal efficiencies reached 28%, 15%, and 8%. Phenanthrene, paranaphthalene, fluoranthene, benzofluoranthene, and benzopyrene removal rates reached 43.3%, 55.5%, 30.6%, 42.9%, and 41.7%, respectively, in the thermal pretreatment system, which were much higher than those in the ultrasound pretreatment and in the control system. Moreover, capillary suction time (CST) of sludge increased after pretreatment, and then reduced after 20 days of anaerobic digestion, indicating that sludge dewaterability was greatly improved after anaerobic digestion. The decrease of protein and polysaccharide in the sludge could improve sludge dewaterability during petrochemical sludge anaerobic digestion. This study suggested that thermal pretreatment might be a promising enhancement method for petrochemical sludge solubilization, thus contributing to degradation of the PAHs, biogas production, and improvement of dewaterability during petrochemical sludge anaerobic digestion. PMID:26327510

Pretreatment methods to improve nerve immunostaining in corneas from long-term fixed embryonic quail eyes

NASA Technical Reports Server (NTRS)

Barrett, J. E.; Wells, D. C.; Conrad, G. W.

1999-01-01

Pretreatment methods were used to improve neurofilament immunostaining in corneas from embryonic day 16 Japanese quail corneas that had been stored in fixative solution for several months. A sequential combination of the following three pretreatments: brief microwave heating in saline, followed by extraction with sodium dodecyl sulfate (SDS) at 37 degrees C, followed by digestion with hyaluronidase at 37 degrees C, produced significantly increased antibody staining of corneal neurofilament proteins, compared with embryonic corneas subjected to no prior pretreatments or to single or two-step protocols. After applying the sequence of all three pretreatments, darkest nerve staining and increased numbers of fine branches were observed, together with lower background staining. Thus, the result of applying the three-step pretreatment sequence is better than that of applying any of its component single pretreatments or even combinations of any two of them. These findings therefore suggest that each of these three pretreatments causes a unique effect, beneficial to immunostaining of neurofilament proteins, and that their individual effects are independent and additive. In addition to embryonic corneas, the three-step procedure also may be useful for immunostaining of nerves in other very delicate, highly-hydrated tissues containing an abundance of extracellular matrix.

Open sun drying of green bean: influence of pretreatments on drying kinetics, colour and rehydration capacity

NASA Astrophysics Data System (ADS)

İsmail, Osman; Kantürk Figen, Aysel; Pişkin, Sabriye

2017-04-01

Green bean ( Phaseolus Vulgaris L), classified under legume family, is a primary source of dietary protein in human diets especially in the agricultural countries. Green bean is susceptible to rapid deterioration because of their high moisture content and in order to prevent and present the green bean drying process is applied. In this study, effects of pretreatments on drying kinetics, colour and rehydration capacity of green bean were investigated. It was observed that the pretreatment affected the drying time. The shortest drying times were obtained from pretreated samples with blanched. Drying times were determined as 47, 41 and 29 h for natural, salted and blanch, respectively. The results showed that pretreatment and ambient temperature significantly ( P = 0.05) affected the drying rate and the drying time. The effective moisture diffusivity was determined by using Fick's second law and was found to be range between 3.15 × 10-10 and 1.2 × 10-10 m2/s for the pre-treated and natural green bean samples. The rehydration values were obtained 2.75, 2.71, 2.29 (g water/g dry matter) for the blanched, salted and natural samples. The effective diffusion coefficients were calculated using the data collected during the falling rate period and the experimental data are fitted to seven thin layer drying models which found in the literature. The Logarithmic model was found to best describe the drying behavior of fresh green beans under open air sun. Rehydration time and color parameters had been determined in order to improve the quality of dried green bean. Regarding with rehydration time and colour data, the best results were obtained at blanched drying conditions.

Effect of dentin biomodifiers on the immediate and long-term bond strengths of a simplified etch and rinse adhesive to dentin.

PubMed

Singh, Payal; Nagpal, Rajni; Singh, Udai Pratap

2017-08-01

This in vitro study evaluated the effect of dentin biomodifiers on the immediate and long-term bond strengths of a simplified etch and rinse adhesive to dentin. Flat coronal dentin surfaces were prepared in 120 extracted human molars. Teeth were randomly divided into 5 groups ( n = 24) according to 5 different surface pre-treatments: No pre-treatment (control); 1M carbodiimide (EDC); 0.1% epigallocatechin-3-gallate (EGCG); 2% minocycline (MI); 10% sodium ascorbate (SA). After surface pre-treatment, adhesive (Adper Single Bond 2 [SB], 3M ESPE) was applied. Composite was applied into transparent plastic tubes (2.5 mm in diameter), which was placed over the bonded dentin surface. From each group, 10 samples were subjected to shear bond strength (SBS) evaluation at 24 hours (immediate) and remaining 10 samples were tested after 6 months (delayed). Additionally, 4 samples per group were subjected to scanning electron microscopic analysis for observation of resin-dentin interface. The data were statistically analysed with Shaperio‑Wilk W test, 2-way analysis of variance (ANOVA), and post hoc Tukey's test. At 24 hours, SBS of all surface pre-treatment groups were comparable with the control group, with significant differences found between EDC and SA groups only ( p = 0.009). After 6 months storage, EDC, EGCG, and MI pre-treatments preserved the resin-dentin bond strength with no significant fall. Dentin pre-treatment with all the dentin biomodifiers except SA resulted in significant preservation of resin-dentin bond over 6 months storage period, without negatively affecting the immediate bond strength of the etch and rinse adhesive tested.

Postharvest Ultrasound-Assisted Freeze-Thaw Pretreatment Improves the Drying Efficiency, Physicochemical Properties, and Macamide Biosynthesis of Maca (Lepidium meyenii).

PubMed

Chen, Jin-Jin; Gong, Peng-Fei; Liu, Yi-Lan; Liu, Bo-Yan; Eggert, Dawn; Guo, Yuan-Heng; Zhao, Ming-Xia; Zhao, Qing-Sheng; Zhao, Bing

2018-04-01

A novel technique of ultrasound-assisted freeze-thaw pretreatment (UFP) was developed to improve the drying efficiency of maca and bioactive amide synthesis in maca. The optimal UFP conditions are ultrasonic processing 90 min at 30 °C with 6 freeze-thaw cycles. Samples with freeze-thaw pretreatment (FP), ultrasound pretreatment (UP), and UFP were prepared for further comparative study. A no pretreatment (NP) sample was included as a control. The results showed that UFP improved the drying efficiency of maca slices, showing the highest effective moisture diffusivity (1.75 × 10 -9 m 2 /s). This result was further supported by low-field nuclear magnetic resonance (LF-NMR) analysis and scanning electron microscopy (SEM). The rehydration capacity and protein content of maca slices were improved by UFP. More importantly, contents of bioactive macamides and their biosynthetic precursors were increased in 2.5- and 10-fold, respectively. In conclusion, UFP is an efficient technique to improve drying efficiency, physicochemical properties, and bioactive macamides of maca, which can be applied in the industrial manufacture of maca products. © 2018 Institute of Food Technologists®.

Supercritical fluids as a green technology for the pretreatment of lignocellulosic biomass.

PubMed

Daza Serna, L V; Orrego Alzate, C E; Cardona Alzate, C A

2016-01-01

One of the main drawbacks for using lignocellulosic biomass is related to its recalcitrance. The pretreatment of lignocellulosic biomass plays an important role for delignification and crystallinity reduction purposes. In this work rice husk (RH) was submitted to supercritical pretreatment at 80°C and 270 bar with the aim to determine the effect on lignin content, crystallinity as well as enzymatic digestibility. The yields obtained were compared with dilute sulfuric acid pretreatment as base case. Additionally a techno-economic and environmental comparison of the both pretreatment technologies was performed. The results show a lignin content reduction up to 90.6% for the sample with 75% moisture content using a water-ethanol mixture. The results for crystallinity and enzymatic digestibility demonstrated that no reductions were reached. Supercritical pretreatment presents the best economical and environmental performance considering the solvents and carbon dioxide recycling. Copyright © 2015 Elsevier Ltd. All rights reserved.

Analysis, fate studies and monitoring of the antifungal agent clotrimazole in the aquatic environment.

PubMed

Peschka, Manuela; Roberts, Paul H; Knepper, Thomas P

2007-10-01

The analysis and presence of clotrimazole, an antifungal agent with logK(OW) > 4, was thoroughly studied in the aquatic environment. For that reason analytical methods based on gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry were developed and validated to quantify clotrimazole with limits of quantification down to 5 and 1 ng/L, respectively. Both methods were compared in an intercalibration exercise. The complete mass-spectrometric fragmentation pattern could be elucidated with the aid of quadrupole time of flight mass spectrometry. Since clotrimazole tends to adsorb to laboratory glassware, studies on its adsorption behaviour were made to ensure the appropriate handling of water samples, e.g. pH, storage time, pretreatment of sampling vessels or material of the vials used for final extracts. The phenomena of adsorption to suspended matter were investigated while analysing different waste-water samples. Application of the methods in various investigated wastewater and surface water samples demonstrated that clotrimazole could only be detected in the low nanogram per litre range of anthropogenic influenced unfiltered water samples after acidification to pH 2.

Cocaine profiling for strategic intelligence, a cross-border project between France and Switzerland: part II. Validation of the statistical methodology for the profiling of cocaine.

PubMed

Lociciro, S; Esseiva, P; Hayoz, P; Dujourdy, L; Besacier, F; Margot, P

2008-05-20

Harmonisation and optimization of analytical and statistical methodologies were carried out between two forensic laboratories (Lausanne, Switzerland and Lyon, France) in order to provide drug intelligence for cross-border cocaine seizures. Part I dealt with the optimization of the analytical method and its robustness. This second part investigates statistical methodologies that will provide reliable comparison of cocaine seizures analysed on two different gas chromatographs interfaced with a flame ionisation detectors (GC-FIDs) in two distinct laboratories. Sixty-six statistical combinations (ten data pre-treatments followed by six different distance measurements and correlation coefficients) were applied. One pre-treatment (N+S: area of each peak is divided by its standard deviation calculated from the whole data set) followed by the Cosine or Pearson correlation coefficients were found to be the best statistical compromise for optimal discrimination of linked and non-linked samples. The centralisation of the analyses in one single laboratory is not a required condition anymore to compare samples seized in different countries. This allows collaboration, but also, jurisdictional control over data.

A simple methodological validation of the gas/particle fractionation of polycyclic aromatic hydrocarbons in ambient air

NASA Astrophysics Data System (ADS)

Kim, Yong-Hyun; Kim, Ki-Hyun

2015-07-01

The analysis of polycyclic aromatic hydrocarbons (PAH) in ambient air requires the tedious experimental steps of both sampling and pretreatment (e.g., extraction or clean-up). To replace pre-existing conventional methods, a simple, rapid, and novel technique was developed to measure gas-particle fractionation of PAH in ambient air based on ‘sorbent tube-thermal desorption-gas chromatograph-mass spectrometer (ST-TD-GC-MS)’. The separate collection and analysis of ambient PAHs were achieved independently by two serially connected STs. The basic quality assurance confirmed good linearity, precision, and high sensitivity to eliminate the need for complicated pretreatment procedures with the detection limit (16 PAHs: 13.1 ± 7.04 pg). The analysis of real ambient PAH samples showed a clear fractionation between gas (two-three ringed PAHs) and particulate phases (five-six ringed PAHs). In contrast, for intermediate (four ringed) PAHs (fluoranthene, pyrene, benz[a]anthracene, and chrysene), a highly systematic/gradual fractionation was established. It thus suggests a promising role of ST-TD-GC-MS as measurement system in acquiring a reliable database of airborne PAH.

Acute d-amphetamine pretreatment does not alter stimulant self-administration in humans.

PubMed

Stoops, William W; Vansickel, Andrea R; Lile, Joshua A; Rush, Craig R

2007-05-01

Recent clinical research indicates that d-amphetamine is effective in treating cocaine and methamphetamine dependence. There is concern, however, with the use of d-amphetamine as a pharmacotherapy because acute administration of d-amphetamine decreases inhibition in cocaine-using individuals and may increase drug-taking behavior. The purpose of the present experiment was to determine whether acute d-amphetamine pretreatment would alter the reinforcing, subject-rated, and cardiovascular effects of d-amphetamine. To this end, 7 human volunteers first sampled doses of oral d-amphetamine (0, 8, and 16 mg). These doses engender moderate drug taking and were selected to avoid a ceiling or floor effect. Volunteers were then allowed to self-administer these sampled doses using a modified progressive-ratio procedure in two sessions in which they received pretreatment with either 0 or 15 mg oral d-amphetamine 2 h prior to completing the modified progressive-ratio procedure. d-Amphetamine produced prototypical stimulant-like effects (e.g., increased ratings of stimulated, elevated blood pressure) and maintained responding on the modified progressive-ratio schedule. Pretreatment with 15 mg oral d-amphetamine also produced prototypical stimulant-like effects, but failed to alter break points for d-amphetamine on the modified progressive-ratio procedure relative to placebo pretreatment. These results indicate that acute d-amphetamine pretreatment does not increase stimulant self-administration.

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yuan, Xueming; Duan, Yonghao; He, Lilin

A systematic study was done to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110 °C for 3 h at biomass loadings of 5, 10, 15, 20 and 25 wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ~25 to 625 Å, enabling assessment of contributions of pores with different sizes to increased porositymore » after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role.« less

A study of degradation resistance and cytocompatibility of super-hydrophobic coating on magnesium.

PubMed

Zhang, Yufen; Feyerabend, Frank; Tang, Shawei; Hu, Jin; Lu, Xiaopeng; Blawert, Carsten; Lin, Tiegui

2017-09-01

Calcium stearate based super-hydrophobic coating was deposited on plasma electrolytic oxidation (PEO) pre-treated magnesium substrate. The pre-treated magnesium and super-hydrophobic coating covered sample were characterized by scanning electron microscopy, X-ray diffraction and electrochemical corrosion measurements. The cytocompatibility and degradation resistance of magnesium, pre-treated magnesium and super-hydrophobic coating were analysed in terms of cell adhesion and osteoblast differentiation. The results indicate that the calcium stearate top coating shows super-hydrophobicity and that the surface is composed of micro/nanostructure. The super-hydrophobic coating covered sample shows higher barrier properties compared with the PEO pre-treated magnesium and bare magnesium. Human osteoblast proliferation, but not differentiation is enhanced by the PEO coating. Contrary, the super-hydrophobic coating reduces proliferation, but enhances differentiation of osteoblast, observable by the formation of hydroxyapatite. The combination of corrosion protection and cell reaction indicates that this system could be interesting for biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering.

PubMed

Yuan, Xueming; Duan, Yonghao; He, Lilin; Singh, Seema; Simmons, Blake; Cheng, Gang

2017-05-01

A systematic study was performed to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110°C for 3h at biomass loadings of 5, 10, 15, 20 and 25wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ∼25 to 625Å, enabling assessment of contributions of pores with different sizes to increased porosity after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role. Copyright © 2017 Elsevier Ltd. All rights reserved.

Sequential high gravity ethanol fermentation and anaerobic digestion of steam explosion and organosolv pretreated corn stover.

PubMed

Katsimpouras, Constantinos; Zacharopoulou, Maria; Matsakas, Leonidas; Rova, Ulrika; Christakopoulos, Paul; Topakas, Evangelos

2017-11-01

The present work investigates the suitability of pretreated corn stover (CS) to serve as feedstock for high gravity (HG) ethanol production at solids-content of 24wt%. Steam explosion, with and without the addition of H 2 SO 4 , and organosolv pretreated CS samples underwent a liquefaction/saccharification step followed by simultaneous saccharification and fermentation (SSF). Maximum ethanol concentration of ca. 76g/L (78.3% ethanol yield) was obtained from steam exploded CS (SECS) with 0.2% H 2 SO 4 . Organosolv pretreated CS (OCS) also resulted in high ethanol concentration of ca. 65g/L (62.3% ethanol yield). Moreover, methane production through anaerobic digestion (AD) was conducted from fermentation residues and resulted in maximum methane yields of ca. 120 and 69mL/g volatile solids (VS) for SECS and OCS samples, respectively. The results indicated that the implementation of a liquefaction/saccharification step before SSF employing a liquefaction reactor seemed to handle HG conditions adequately. Copyright © 2017 Elsevier Ltd. All rights reserved.

Low-temperature, Low-Energy, and High-Efficiency Pretreatment Technology for Large Wood Chips with a Redox Couple Catalyst.

PubMed

Gogoi, Parikshit; Zhang, Zhe; Geng, Zhishuai; Liu, Wei; Hu, Weize; Deng, Yulin

2018-03-22

The pretreatment of lignocellulosic biomass plays a vital role in the conversion of cellulosic biomass to bioethanol, especially for softwoods and hardwoods. Although many pretreatment technologies have been reported so far, only a few pretreatment methods can handle large woodchips directly. To improve the efficiency of pretreatment, existing technologies require the grinding of the wood into small particles, which is an energy-consuming process. Herein, for the first time, we report a simple, effective, and low-temperature (≈100 °C) process for the pretreatment of hardwood (HW) and softwood (SW) chips directly by using a catalytic system of FeCl 3 /NaNO 3 (FCSNRC). The pretreatment experiments were conducted systematically, and a conversion of 71.53 and 70.66 % of cellulose to sugar could be obtained for the direct use of large HW and SW chips. The new method reported here overcomes one of the critical barriers in biomass-to-biofuel conversion, and both grinding and thermal energies can be reduced significantly. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Review of the Extraction and Determination Methods of Thirteen Essential Vitamins to the Human Body: An Update from 2010.

PubMed

Zhang, Yuan; Zhou, Wei-E; Yan, Jia-Qing; Liu, Min; Zhou, Yu; Shen, Xin; Ma, Ying-Lin; Feng, Xue-Song; Yang, Jun; Li, Guo-Hui

2018-06-19

Vitamins are a class of essential nutrients in the body; thus, they play important roles in human health. The chemicals are involved in many physiological functions and both their lack and excess can put health at risk. Therefore, the establishment of methods for monitoring vitamin concentrations in different matrices is necessary. In this review, an updated overview of the main pretreatments and determination methods that have been used since 2010 is given. Ultrasonic assisted extraction, liquid⁻liquid extraction, solid phase extraction and dispersive liquid⁻liquid microextraction are the most common pretreatment methods, while the determination methods involve chromatography methods, electrophoretic methods, microbiological assays, immunoassays, biosensors and several other methods. Different pretreatments and determination methods are discussed.

Evaluation of pretreatment methods on mixed inoculum for both batch and continuous thermophilic biohydrogen production from cassava stillage.

PubMed

Luo, Gang; Xie, Li; Zou, Zhonghai; Wang, Wen; Zhou, Qi

2010-02-01

Anaerobic sludges, pretreated by chloroform, base, acid, heat and loading-shock, as well as untreated sludge were evaluated for their thermophilic fermentative hydrogen-producing characters from cassava stillage in both batch and continuous experiments. Results showed that the highest hydrogen production was obtained by untreated sludge and there were significant differences (p<0.05) in hydrogen yields (varied from 32.9 to 65.3mlH(2)/gVS) among the tested pretreatment methods in batch experiments. However, the differences in hydrogen yields disappeared in continuous experiments, which indicated the pretreatment methods had only short-term effects on the hydrogen production. Further study showed that alkalinity was a crucial parameter influencing the fermentation process. When the influent was adjusted to pH 6 by NaHCO(3) instead of NaOH, the hydrogen yield increased from about 40 to 52mlH(2)/gVS in all the experiments. Therefore, pretreatment of anaerobic sludge is unnecessary for practical thermophilic fermentative hydrogen production from cassava stillage.

Effect of aerobic pre-treatment on hydrogen and methane production in a two-stage anaerobic digestion process using food waste with different compositions.

PubMed

Rafieenia, Razieh; Girotto, Francesca; Peng, Wei; Cossu, Raffaello; Pivato, Alberto; Raga, Roberto; Lavagnolo, Maria Cristina

2017-01-01

Aerobic pre-treatment was applied prior to two-stage anaerobic digestion process. Three different food wastes samples, namely carbohydrate rich, protein rich and lipid rich, were prepared as substrates. Effect of aerobic pre-treatment on hydrogen and methane production was studied. Pre-aeration of substrates showed no positive impact on hydrogen production in the first stage. All three categories of pre-aerated food wastes produced less hydrogen compared to samples without pre-aeration. In the second stage, methane production increased for aerated protein rich and carbohydrate rich samples. In addition, the lag phase for carbohydrate rich substrate was shorter for aerated samples. Aerated protein rich substrate yielded the best results among substrates for methane production, with a cumulative production of approximately 351ml/gVS. With regard to non-aerated substrates, lipid rich was the best substrate for CH 4 production (263ml/gVS). Pre-aerated P substrate was the best in terms of total energy generation which amounted to 9.64kJ/gVS. This study revealed aerobic pre-treatment to be a promising option for use in achieving enhanced substrate conversion efficiencies and CH 4 production in a two-stage AD process, particularly when the substrate contains high amounts of proteins. Copyright © 2016 Elsevier Ltd. All rights reserved.

Technological pretreatment of the synchysite non-oxidized ore

NASA Astrophysics Data System (ADS)

Munkhtsetseg, B.; Burmaa, G.

2013-06-01

Mongolia has rich deposits of rare, precious, and poly-metallic ores. Nowadays, it is important to research separation of rare earth elements oxides concentrates from the ores, analyze their unique physical chemical characteristics, and purified it. Our investigation on raw materials focuses on rare earth non-oxidized ores. Main mineral in this rock sample is Synchysite (LnCa(CO3)2F. We did technological and thermal pretreatment: direct sulphurization (H2SO4), sulphurization with subsequent roasting (800°C+H2SO4), sulphurization prior to roasting (H2SO4+650°C). Sulphurization method based on dissolution of rare earth mineral into sulfuric acid (93%) according to the reaction. The amount of rare earth element oxides is almost 10 times greater (29.16%) after direct sulphurization process, almost 8 times greater (21.14%) after sulphurization with subsequent roasting, and almost 20 times greater (44.62%) after sulphurization prior to roasting process. After those technological pretreatment raw material's micro elements Thorium and Uranium contents are reduced as follows: H2SO4>800°C+H2SO4>H2SO4+650°C. These results show that cerium group rare earth elements have very good solubility in water at +2°C temperature and decreasing micro elements content uranium and thorium good pretreatment condition is prior to roasting (H2SO4+650°C) of synchysite non-oxidized ore.

Fungal leaching of valuable metals from a power plant residual ash using Penicillium simplicissimum: Evaluation of thermal pretreatment and different bioleaching methods.

PubMed

Rasoulnia, P; Mousavi, S M; Rastegar, S O; Azargoshasb, H

2016-06-01

Each year a tremendous volume of V-Ni rich ashes is produced by fuel oil consuming power plants throughout the world. Recovery of precious metals existing in these ashes is very important from both economic and environmental aspects. The present research was aimed at investigating bioleaching potential of Penicillium simplicissimum for the recovery of metals from power plant residual ash (PPR ash) using different bioleaching methods such as one-step, two-step, and spent-medium bioleaching at 1% (w/v) pulp density. Furthermore, the effects of thermal pretreatment on leaching of V, Ni, and Fe, as major elements present in PPR ash, were studied. Thermal pretreatment at various temperatures removed the carbonaceous and volatile fraction of the ash and affected the fungal growth and metal leachability. The highest extraction yields of V and Ni were achieved for the original PPR ash, using spent-medium bioleaching in which nearly 100% of V and 40% of Ni were extracted. The maximum extraction yield of Fe (48.3%) was obtained for the pretreated PPR ash at 400°C by spent-medium bioleaching. In addition, the fungal growth in pure culture was investigated through measurement of produced organic acids via high performance liquid chromatography (HPLC). Chemical leaching experiments were performed, using commercial organic acids at the same concentrations as those produced under optimum condition of fungal growth (5237ppm citric, 3666ppm gluconic, 1287ppm oxalic and 188ppm malic acid). It was found that in comparison to chemical leaching, bioleaching improved V and Ni recovery up to 19% and 12%, respectively. Moreover, changes in physical and chemical properties as well as morphology of the samples utilizing appropriate analytical methods such as XRF, XRD, FTIR, and FE-SEM were comprehensively investigated. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of osmotic dehydration pretreatment and glassy state storage on the quality attributes of frozen mangoes under long-term storage.

PubMed

Zhao, Jin-Hong; Xiao, Hong-Wei; Ding, Yang; Nie, Ying; Zhang, Yu; Zhu, Zhen; Tang, Xuan-Ming

2017-05-01

Changes in the quality of frozen mango cuboids were investigated during long-term glassy state storage with and without osmotic dehydration pretreatment. The mango cuboids were dehydrated in mixed solutions (sucrose: glucose: fructose in a ratio of 3.6:1:3) of different concentrations (30, 40, and 50% (wt/wt)) prior to freezing and then stored at -55 °C (in the glassy state) for 6 months. The results revealed that compared with the untreated samples, osmotic pretreatment decreased total color difference (reduced by 15.6-62.3%), drip loss (reduced by 8.2-29.5%) and titration acidity (reduced by 1.3-9.4%), while increasing hardness (increased by 48.8-82.3%), vitamin C content (increased by 72.5-120.6%) and total soluble solids (increased by 21.8-53.7%) of frozen mangoes after 6 months. Dehydration with a sugar concentration of 40% was considered as the optimal pretreatment condition. In addition, a storage temperature of -55 °C provided better retention of quality than rubbery state storage at -18 °C. With prolonged storage time, the quality of frozen mangoes continued to change, even in the glassy state. However, the changes in quality of the osmotic-dehydrated samples were less than those of the untreated samples. The current work indicates that osmotic pretreatment and glassy state storage significantly improved the quality of frozen mangoes during long-term storage.

Comparative study of SPORL and dilute-acid pretreatments of spruce for cellulosic ethanol production

Treesearch

L. Shuai; Q. Yang; Junyong Zhu; F.C. Lu; P.J. Weimer; J. Ralph; X.L. Pan

2010-01-01

The performance of two pretreatment methods, sulfite pretreatment to overcome recalcitrance of lignocelluloses (SPORL) and dilute acid (DA), was compared in pretreating softwood (spruce) for fuel ethanol production at 180C for 30 min with a sulfuric acid loading of 5% on oven-dry wood and a 5:1 liquor to-wood ratio. SPORL was supplemented with 9% sodium...

Application of partial least squares near-infrared spectral classification in diabetic identification

NASA Astrophysics Data System (ADS)

Yan, Wen-juan; Yang, Ming; He, Guo-quan; Qin, Lin; Li, Gang

2014-11-01

In order to identify the diabetic patients by using tongue near-infrared (NIR) spectrum - a spectral classification model of the NIR reflectivity of the tongue tip is proposed, based on the partial least square (PLS) method. 39sample data of tongue tip's NIR spectra are harvested from healthy people and diabetic patients , respectively. After pretreatment of the reflectivity, the spectral data are set as the independent variable matrix, and information of classification as the dependent variables matrix, Samples were divided into two groups - i.e. 53 samples as calibration set and 25 as prediction set - then the PLS is used to build the classification model The constructed modelfrom the 53 samples has the correlation of 0.9614 and the root mean square error of cross-validation (RMSECV) of 0.1387.The predictions for the 25 samples have the correlation of 0.9146 and the RMSECV of 0.2122.The experimental result shows that the PLS method can achieve good classification on features of healthy people and diabetic patients.

Direct and simultaneous determination of representative byproducts in a lignocellulosic hydrolysate of corn stover via gas chromatography-mass spectrometry with a Deans switch.

PubMed

Zheng, Rongping; Zhang, Hongman; Zhao, Jing; Lei, Mingliu; Huang, He

2011-08-05

Pretreatment is one of the most important steps in producing fuel ethanol from lignocellulosic biomass. Simple, fast and accurate quantification of byproducts in lignocellulosic hydrolysates is critical to optimize the pretreatment procedures, but still a challenge. In this paper, a new GC-MS (SIM) method based on a Deans switch has been developed for the determination of byproducts in a corn stover hydrolysate. The Deans switch was incorporated into a hardware system that facilitated the direct aqueous injection (DAI) on GC-MS system. Simultaneous chromatographic separation and quantification of 18 byproducts including four aliphatic acids, five furan derivatives, four phenolic compounds and five others were achieved within 45 min. The detection limits of the presented method for various byproducts were in the range of 0.007-0.832 mg/L. The within-day and between-day precisions of the method were less than 6.0% (RSD, n=6). The accuracy of the method was confirmed with recoveries of 86-128%. A lignocellulosic hydrolysate sample of corn stover was successfully analyzed using this method, with aliphatic acids and furan derivatives accounting for 89.15% of the selected total byproducts. Copyright © 2011 Elsevier B.V. All rights reserved.

Solid phase microextraction and gas chromatography-mass spectrometry methods for residual solvent assessment in seized cocaine and heroin.

PubMed

Cabarcos, Pamela; Herbello-Hermelo, Paloma; Álvarez-Freire, Iván; Moreda-Piñeiro, Antonio; Tabernero, María Jesús; Bermejo, Ana María; Bermejo-Barrera, Pilar

2016-09-01

A simple sample pre-treatment method based on solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized and validated for the assessment of 15 residual solvents (2-propanol, 2-methylpentane, 3-methylpentane, acetone, ethyl acetate, benzene, hexane, methylcyclohexane, methylcyclopentane, m-xylene, propyl acetate, toluene, 1,2,4-trimethylbenzene, dichloromethane, and ethylbenzene) in seized illicit cocaine and heroin. DMSO and DMF as sample diluents were found to offer the best residual solvent transference to the head space for further adsorption onto the SPME fiber, and the developed method therefore showed high sensitivity and analytical recovery. Variables affecting SPME were fully evaluated by applying an experimental design approach. Best conditions were found when using an equilibration time of 5 min at 70 °C and headspace sampling of residual solvents at the same temperature for 15 min. Method validation, performed within the requirements of international guidelines, showed excellent sensitivity, as well as intra- and inter-day precision and accuracy. The proposed methodology was applied to 96 cocaine samples and 14 heroin samples seized in Galicia (northwestern Spain) within 2013 and 2014.

Heat-assisted aqueous extraction of rice flour for arsenic speciation analysis.

PubMed

Narukawa, Tomohiro; Chiba, Koichi

2010-07-28

A versatile heat-assisted pretreatment aqueous extraction method for the analysis of arsenic species in rice was developed. Rice flour certified reference materials NIST SRM1568a and NMIJ CRM 7503-a and a flour made from polished rice were used as samples, and HPLC-ICP-MS was employed for the determination of arsenic species. Arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) were detected in NIST SRM, and As(III), As(V) and DMAA were found in NMIJ CRM and the prepared polished rice flour. The sums of the concentrations of all species in each rice flour sample were 97-102% of the total arsenic concentration in each sample.

Effect of White Charcoal on COD Reduction in Wastewater Treatment

NASA Astrophysics Data System (ADS)

Pijarn, Nuchanaporn; Butsee, Manipa; Buakul, Kanokwan; Seng, Hasan; Sribuarai, Tinnphat; Phonprasert, Pongtep; Taneeto, Kla; Atthameth, Prasertsil

2017-06-01

The objective of this study is to compare the COD reduction in wastewater between using coconut shell and coconut spathe white charcoal from Khlong Wat NongPra-Ong, Krathumbaen, SamutSakhon province, Thailand. The waste water samples were collected using composite sampling method. The experimental section can be divided into 2 parts. The first part was study the optimum of COD adsorption time using both white charcoals. The second part was study the optimum amount of white charcoal for chemical oxygen demand (COD) reduction. The pre-treatment of wastewater was examined in parameters include temperature, alkalinity (pH), conductivity, turbidity, suspended solid (SS), total dissolved solid (TDS), and COD. The results show that both white charcoals can reduce COD of wastewater. The pH of pre-treatment wastewater had pH 9 but post-treatment wastewaters using both white charcoals have pH 8. The COD of pre-treatment wastewater had COD as 258 mg/L but post-treatment wastewater using coconut shell white charcoal had COD steady at 40 mg/L in 30 min and the amount of white charcoals 4 g. The COD of post-treatment wastewater using coconut spathe white charcoal had COD steady at 71 mg/L in 30 min and the amount of white charcoals 4 g. Therefore comparison of COD reduction between coconut shell white charcoal versus coconut spathe white charcoal found that the coconut shell white charcoal had efficiency for COD reduction better than coconut spathe white charcoal.

Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

PubMed

Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

2016-03-25

Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples, respectively. The complementary of both chromatographic modes was also demonstrated, as ME was observed only scarcely for urine and plasma samples when selecting the most appropriate chromatographic mode. Copyright © 2015 Elsevier B.V. All rights reserved.

Efficiency of pretreatment of aqueous samples using a macroporous strong anion-exchange resin on the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry after tert.-butyldimethylsilylation.

PubMed

Kataoka, M; Tsuge, K; Seto, Y

2000-09-08

A pretreatment procedure, using a macroporous strong anion-exchange resin (MSA) has been established for the determination of nerve gas hydrolysis products by gas chromatography-mass spectrometry (GC-MS) after tert.-butyldimethylsilyl (TBDMS) derivatization. Aqueous solutions of methylphosphonic acid (MPA) and three alkyl methylphosphonic acids (AMPAs) (ethyl, isopropyl and pinacolyl methylphosphonic acid), were retained on the MSA column, and then quantitatively eluted with 0.1 M hydrochloric acid. The neutralized column eluate was dried, and MPA and AMPAs were derivatized with N-methyl-N-(tert.-butyldimethylsilyl)-trifluoroacetamide and analyzed by GC-MS. The column eluate was also analyzed in order to determine the exact hydrolysis product levels by capillary electrophoresis using borate and benzoate buffer (pH 6). The MSA pretreatment was examined for the clean-up of aqueous extracts of three types of soils and an aqueous solution containing 10% sucrose, which is regarded as model for a typical soft drink, after spiking with MPA and AMPAs. MPA and AMPAs were quantitatively recovered in the MSA eluate fraction from those samples, except for MPA from volcanic acid and alluvial soils. The yields of TBDMS derivatives were remarkably improved, compared with for which no pretreatment was used and also for those in which a strong cation-exchange resin was used. The achieved detection limits of MPA and AMPAs ranged from 0.12 to 0.18 microg/g of soil (S/N=3). The established MSA method was applied to the pretreatment of spiked sea water, two types of beverages, Pepsi Cola and canned coffee. Although the yields of TBDMS derivatives of MPA and AMPAs in sea water (in a range between 44 and 96%) and AMPAs in Pepsi Cola (in a range between 58 and 92%) were rather high, those for MPA in the Pepsi Cola (27%) and those for MPA and AMPAs in the canned coffee (in a range between 5 and 17%) were low.

Measurement of trace nitrate concentrations in seawater by ion chromatography with valve switching

NASA Astrophysics Data System (ADS)

Du, Juan; Fa, Yun; Zheng, Yue; Li, Xuebing; Du, Fanglin; Yang, Haiyan

2014-05-01

An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity ( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability (RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.

Effect of structural changes of lignocelluloses material upon pre-treatment using green solvents

NASA Astrophysics Data System (ADS)

Gunny, Ahmad Anas Nagoor; Arbain, Dachyar; Jamal, Parveen

2017-04-01

The Malaysia Biomass strategy 2020 stated that the key step of biofuel production from biomass lies on the pretreatment process. Conventional `pre-treatment' methods are `non-green" and costly. The recent green and cost-effective biomass pretreatment is using new generation of Ionic Liquids also known as Deep Eutectic Solvents (DESs). DESs are made of renewable components are cheaper, greener and the process synthesis are easier. Thus, the present paper concerns with the preparation of various combination of DES and to study the effect of DESs pretreatment process on microcrystalline cellulose (MCC), a model substrate. The crystalline structural changes were studied using using X-ray Diffraction Methods, Fourier Transformed Infrared Spectroscopy (FTIR) and surface area and pore size analysis. Results showed reduction of crystalline structure of MCC treated with the DESs and increment of surface area and pore size of MCC after pre-treatment process. These results indicated the DES has successfully converted the lignocelluloses material in the form suitable for hydrolysis and conversion to simple sugar.

Breakdown of cell wall nanostructure in dilute acid pretreated biomass.

PubMed

Pingali, Sai Venkatesh; Urban, Volker S; Heller, William T; McGaughey, Joseph; O'Neill, Hugh; Foston, Marcus; Myles, Dean A; Ragauskas, Arthur; Evans, Barbara R

2010-09-13

The generation of bioethanol from lignocellulosic biomass holds great promise for renewable and clean energy production. A better understanding of the complex mechanisms of lignocellulose breakdown during various pretreatment methods is needed to realize this potential in a cost and energy efficient way. Here we use small-angle neutron scattering (SANS) to characterize morphological changes in switchgrass lignocellulose across molecular to submicrometer length scales resulting from the industrially relevant dilute acid pretreatment method. Our results demonstrate that dilute acid pretreatment increases the cross-sectional radius of the crystalline cellulose fibril. This change is accompanied by removal of hemicellulose and the formation of R(g) ∼ 135 A lignin aggregates. The structural signature of smooth cell wall surfaces is observed at length scales larger than 1000 A, and it remains remarkably invariable during pretreatment. This study elucidates the interplay of the different biomolecular components in the breakdown process of switchgrass by dilute acid pretreatment. The results are important for the development of efficient strategies of biomass to biofuel conversion.

Improving production of volatile fatty acids from food waste fermentation by hydrothermal pretreatment.

PubMed

Yin, Jun; Wang, Kun; Yang, Yuqiang; Shen, Dongsheng; Wang, Meizhen; Mo, Han

2014-11-01

Food waste (FW) was pretreated by a hydrothermal method and then fermented for volatile fatty acid (VFAs) production. The soluble substance in FW increased after hydrothermal pretreatment (⩽200 °C). Higher hydrothermal temperature would lead to mineralization of the organic compounds. The optimal temperature for organic dissolution was 180 °C, at which FW dissolved 42.5% more soluble chemical oxygen demand than the control. VFA production from pretreated FW fermentation was significantly enhanced compared with the control. The optimal hydrothermal temperature was 160 °C with a VFA yield of 0.908 g/g VSremoval. Butyrate and acetate were the prevalent VFAs followed by propionate and valerate. FW fermentation was inhibited after 200 °C pretreatment. The VFAs were extracted from the fermentation broth by liquid-liquid extraction. The VFA recovery was 50-70%. Thus, 0.294-0.411 g VFAs could be obtained per gram of hydrothermally pretreated FW (in dry weight) by this method. Copyright © 2014 Elsevier Ltd. All rights reserved.

Ethanol production from poplar wood through enzymatic saccharification and fermentation by dilute acid and SPORL pretreatments

Treesearch

Z.J. Wang; J.Y. Zhu; Ronald S. Jr. Zalesny; K.F. Chen

2012-05-01

Dilute acid (DA) and Sulfite Pretreatment to Overcome Recalcitrance of Lignocelluloses (SPORL) pretreatments were directly applied to wood chips of four poplar wood samples of different genotypes (hereafter referred to as poplars; Populus tremuloides Michx. ‘native aspen collection’; Populus deltoides Bartr. ex Marsh x Populus nigra L. ‘NE222’ and ‘DN5’; P. nigra x...

Pre-treatment Drug Use Characteristics and Experiences among Patients in a Voluntary Substance Abuse Treatment Center in Malaysia: A Mixed Methods Approach

PubMed Central

Krishnan, Archana; Brown, Shan-Estelle; Ghani, Mansur; Khan, Farrah; Kamarulzaman, Adeeba; Altice, Frederick L.

2017-01-01

Background Drug use in Malaysia remains a significant public health and social problem despite implementation of harsh punitive drug policies such as forcibly placing suspected drug users into compulsory drug detention centers (CDDCs). Following criticism over human right violations in CDDCs, Malaysia has begun to transition towards voluntary drug treatment centers known as Cure & Care (C&C) Centers. To best serve the needs of regional C&Cs, data on drug use are essential among patients accessing treatment. Using a mixed methods approach, we examined pre-treatment drug use characteristics and experiences with addiction treatment among C&C patients in Kelantan – a religiously conservative state in Northeast Malaysia with high prevalence of drug use but where limited data are available on drug use patterns. Methods A mixed methods study utilizing surveys (N=96) and semi-structured interviews (N=20) was conducted among a convenience sample of inpatients and outpatients at the Pengkalan Chepa C&C Center in Kelantan. Results Survey results showed 89.6% of participants met screening criteria for moderate to severe addiction severity. Nearly 90% reported lifetime illicit amphetamine (syabu, meth, ice, and pil kuda) use followed by alcohol (60.4%) and opioids (52.1%). Qualitative results pointed to the powerful influence of peer networks in drug initiation and relapse, and the positive effect of the C&C on drug rehabilitation. Conclusions The drug use profile of the Kelantan C&C enrollees shows extensive pre-treatment amphetamine use, polysubstance use, and injection drug use including high-risk behaviors such as sharing needles, syringes and containers. Evidence points to the need for integration of social support-oriented practices and behavioral interventions into the rehabilitation of drug users in this region. PMID:26914230

Application and optimization of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for sensitive determination of polyamines in turkey breast meat samples.

PubMed

Bashiry, Moein; Mohammadi, Abdorreza; Hosseini, Hedayat; Kamankesh, Marzieh; Aeenehvand, Saeed; Mohammadi, Zaniar

2016-01-01

A novel method based on microwave-assisted extraction and dispersive liquid-liquid microextraction (MAE-DLLME) followed by high-performance liquid chromatography (HPLC) was developed for the determination of three polyamines from turkey breast meat samples. Response surface methodology (RSM) based on central composite design (CCD) was used to optimize the effective factors in DLLME process. The optimum microextraction efficiency was obtained under optimized conditions. The calibration graphs of the proposed method were linear in the range of 20-200 ng g(-1), with the coefficient determination (R(2)) higher than 0.9914. The relative standard deviations were 6.72-7.30% (n = 7). The limits of detection were in the range of 0.8-1.4 ng g(-1). The recoveries of these compounds in spiked turkey breast meat samples were from 95% to 105%. The increased sensitivity in using the MAE-DLLME-HPLC-UV has been demonstrated. Compared with previous methods, the proposed method is an accurate, rapid and reliable sample-pretreatment method. Copyright © 2015 Elsevier Ltd. All rights reserved.

Human Mesenchymal Stem Cells Pretreated with Interleukin-1β and Stimulated with Bone Morphogenetic Growth Factor-3 Enhance Chondrogenesis.

PubMed

Hingert, Daphne; Barreto Henriksson, Helena; Brisby, Helena

2018-05-01

Low back pain is one of the most common ailments in western countries afflicting more than 80% of the population, and the main cause is considered to be degeneration of intervertebral discs. Interleukin-1β (IL-1β) is a vital inflammatory cytokine found in abundance in degenerated disc environment, whereas bone morphogenetic growth factor-3 (BMP-3) is believed to promote chondrogenesis through transforming growth factor-beta (TGF-β) pathway. The aim was to study the effects of BMP-3, IL-1β, and combination (pretreatment with IL-1β) on human mesenchymal stem cells (hMSCs) encapsulated in PuraMatrix™ hydrogel (Phg) especially in the absence of TGF-β in order to investigate the proliferation and differentiation ability of hMSCs over 28-day period. One hundred microliters of hMSCs' cell suspension was encapsulated between two layers of 100 μL hydrogels forming a sandwich-like structure. The encapsulated hMSCs were cultured in two sets of media, chondrogenic (C) and nonchondrogenic (nC) media, along with addition of BMP-3 (10 ng/mL) and IL-1β (10 ng/mL). To study the combined effects of BMP-3 and IL-1β, the encapsulated hMSCs were first pretreated with relevant media containing IL-1β for 24 h, and then the media was replaced by media containing BMP-3 for the remaining experimental time period. IL-1β pretreatment was carried out in both C and nC media. The samples were collected at day 7, 14, and 28. Proliferation and differentiation of hMSCs into chondrocyte-like cells were observed in all samples. Proteoglycan accumulation was observed in pretreatment samples in C media. The protein and gene expression of Sox-9 and COL2A1, respectively, showed the occurrence of chondrogenesis in all samples. High cell viability, proliferation, and differentiation were achieved in this in vitro model confirming that BMP-3 alone in the absence of TGF-β could drive hMSCs into chondrogenic lineage. Pretreatment with IL-1β followed by BMP-3 stimulation resulted in high proteoglycan accumulation compared to stimulation with growth factors or cytokine alone. This suggests that pretreatment with a pro-inflammatory cytokine before driving them into a chondrogenic lineage might be of importance also in vivo.

SEM/XPS analysis of fractured adhesively bonded graphite fibre-reinforced polyimide composites

NASA Technical Reports Server (NTRS)

Devilbiss, T. A.; Messick, D. L.; Wightman, J. P.; Progar, D. J.

1985-01-01

The surfaces of the graphite fiber-reinforced polyimide composites presently pretreated prior to bonding with polyimide adhesive contained variable amounts of a fluoropolymer, as determined by X-ray photoelectron spectroscopy. Lap shear strengths were determined for unaged samples and for those aged over 500- and 1000-hour periods at 177 and 232 C. Unaged sample lap strengths, which were the highest obtained, exhibited no variation with surface pretreatment, but a significant decrease is noted with increasing aging temperature. These thermally aged samples, however, had increased surface fluorine concentration, while a minimal concentration was found in unaged samples. SEM demonstrated a progressive shift from cohesive to adhesive failure for elevated temperature-aged composites.

Electrochemical pretreatment of waste activated sludge: effect of process conditions on sludge disintegration degree and methane production.

PubMed

Ye, Caihong; Yuan, Haiping; Dai, Xiaohu; Lou, Ziyang; Zhu, Nanwen

2016-11-01

Waste activated sludge (WAS) requires a long digestion time because of a rate-limiting hydrolysis step - the first phase of anaerobic digestion (AD). Pretreatment can be used prior to AD to facilitate the hydrolysis step and improve the efficiency of WAS digestion. This study evaluated a novel application of electrochemical (EC) technology employed as the pretreatment method prior to AD of WAS, focusing on the effect of process conditions on sludge disintegration and subsequent AD process. A superior process condition of EC pretreatment was obtained by reaction time of 30 min, electrolysis voltage of 20 V, and electrode distance of 5 cm, under which the disintegration degree of WAS ranged between 9.02% and 9.72%. In the subsequent batch AD tests, 206 mL/g volatile solid (VS) methane production in EC pretreated sludge was obtained, which was 20.47% higher than that of unpretreated sludge. The AD time was 19 days shorter for EC pretreated sludge compared to the unpretreated sludge. Additionally, the EC + AD reactor achieved 41.84% of VS removal at the end of AD. The analysis of energy consumption showed that EC pretreatment could be effective in enhancing sludge AD with reduced energy consumption when compared to other pretreatment methods.

Temperature phased anaerobic digestion increases apparent hydrolysis rate for waste activated sludge.

PubMed

Ge, Huoqing; Jensen, Paul D; Batstone, Damien J

2011-02-01

It is well established that waste activated sludge with an extended sludge age is inherently slow to degrade with a low extent of degradation. Pre-treatment methods can be used prior to anaerobic digestion to improve the efficiency of activated sludge digestion. Among these pre-treatment methods, temperature phased anaerobic digestion (TPAD) is one promising method with a relatively low energy input and capital cost. In this study, an experimental thermophilic (50-70 °C)-mesophilic system was compared against a control mesophilic-mesophilic system. The thermophilic-mesophilic system achieved 41% and 48% volatile solids (VS) destruction during pre-treatment of 60 °C and 65 °C (or 70 °C) respectively, compared to 37% in the mesophilic-mesophilic TPAD system. Solubilisation in the first stage was enhanced during thermophilic pre-treatment (15% at 50 °C and 27% at 60 °C, 65 °C and 70 °C) over mesophilic pre-treatment (7%) according to a COD balance. This was supported by ammonia-nitrogen measurements. Model based analysis indicated that the mechanism for increased performance was due to an increase in hydrolysis coefficient under thermophilic pre-treatment of 60 °C (0.5 ± 0.1 d(-1)), 65 °C (0.7 ± 0.2 d(-1)) and 70 °C (0.8 ± 0.2 d(-1)) over mesophilic pre-treatment (0.2 ± 0.1 d(-1)), and thermophilic pre-treatment at 50 °C (0.12 ± 0.06 d(-1)). © 2010 Elsevier Ltd. All rights reserved.

Xylanase supplementation on enzymatic saccharification of dilute acid pretreated poplars at different severities

Treesearch

Chao Zhang; Xinshu Zhuang; Zhao Jiang Wang; Fred Matt; Franz St. John; J.Y. Zhu

2013-01-01

Three pairs of solid substrates from dilute acid pretreatment of two poplar wood samples were enzymatically hydrolyzed by cellulase preparations supplemented with xylanase. Supplementation of xylanase improved cellulose saccharification perhaps due to improved cellulose accessibility by xylan hydrolysis. Total xylan removal directly affected enzymatic cellulose...

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1989-01-01

Chapter Al of the laboratory manual contains methods used by the U.S. Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, the total recoverable and total of constituents in water-suspended sediment samples, and the recoverable and total concentrations of constituents in samples of bottom material. The introduction to the manual includes essential definitions and a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including the accuracy and precision of analyses, the use of standard-reference water samples, and the operation of an effective quality-assurance program. Methods for sample preparation and pretreatment are given also. A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods of these techniques are arranged alphabetically by constituent. For each method, the general topics covered are the application, the principle of the method, the interferences, the apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 126 methods are given for the determination of 70 inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1985-01-01

Chapter Al of the laboratory manual contains methods used by the Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, total recoverable and total of constituents in water-suspended sediment samples, and recoverable and total concentrations of constituents in samples of bottom material. Essential definitions are included in the introduction to the manual, along with a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including accuracy and precision of analyses, the use of standard reference water samples, and the operation of an effective quality assurance program. Methods for sample preparation and pretreatment are given also.A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods involving these techniques are arranged alphabetically according to constituent. For each method given, the general topics covered are application, principle of the method, interferences, apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 125 methods are given for the determination of 70 different inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Hydrothermal pre-treatment of rapeseed straw.

PubMed

Díaz, Manuel J; Cara, Cristóbal; Ruiz, Encarnación; Romero, Inmaculada; Moya, Manuel; Castro, Eulogio

2010-04-01

As a first step for ethanol production from alternative raw materials, rapeseed straw was studied for fermentable sugar production. Liquid hot water was used as a pre-treatment method and the influence of the main pre-treatment variables was assessed. Experimental design and response surface methodology were applied using pre-treatment temperature and process time as factors. The pretreated solids were further submitted to enzymatic hydrolysis and the corresponding yields were used as pre-treatment performance evaluation. Liquid fractions obtained from pre-treatment were also characterized in terms of sugars and no-sugar composition. A mathematical model describing pre-treatment effects is proposed. Results show that enzymatic hydrolysis yields near to 100% based on pretreated materials can be achieved at 210-220 degrees C for 30-50 min, equivalent to near 70% of glucose present in the raw material. According to the mathematical model, a softer pre-treatment at 193 degrees C for 27 min results in 65% of glucose and 39% of xylose available for fermentation. Copyright 2009 Elsevier Ltd. All rights reserved.

Development of PMA real-time PCR method to quantify viable cells of Pantoea agglomerans CPA-2, an antagonist to control the major postharvest diseases on oranges.

PubMed

Soto-Muñoz, Lourdes; Teixidó, Neus; Usall, Josep; Viñas, Inmaculada; Crespo-Sempere, Ana; Torres, Rosario

2014-06-16

Dilution plating is the quantification method commonly used to estimate the population level of postharvest biocontrol agents, but this method does not permit a distinction among introduced and indigenous strains. Recently, molecular techniques based on DNA amplification such as quantitative real-time PCR (qPCR) have been successfully applied for their high strain-specific detection level. However, the ability of qPCR to distinguish viable and nonviable cells is limited. A promising strategy to avoid this issue relies on the use of nucleic acid intercalating dyes, such as propidium monoazide (PMA), as a sample pretreatment prior to the qPCR. The objective of this study was to optimize a protocol based on PMA pre-treatment samples combined with qPCR to distinguish and quantify viable cells of the biocontrol agent P. agglomerans CPA-2 applied as a postharvest treatment on orange. The efficiency of PMA-qPCR method under the established conditions (30μM PMA for 20min of incubation followed by 30min of LED light exposure) was evaluated on an orange matrix. Results showed no difference in CFU or cells counts of viable cells between PMA-qPCR and dilution plating. Samples of orange matrix inoculated with a mixture of viable/dead cells showed 5.59log10 CFU/ml by dilution plating, 8.25log10 cells/ml by qPCR, and 5.93log10 cells/ml by PMA-qPCR. Furthermore, samples inoculated with heat-killed cells were not detected by dilution plating and PMA-qPCR, while by qPCR was of 8.16log10 cells/ml. The difference in quantification cycles (Cq) among qPCR and PMA-qPCR was approximately 16cycles, which means a reduction of 65,536 fold of the dead cells detected. In conclusion, PMA-qPCR method is a suitable tool for quantify viable CPA-2 cells, which could be useful to estimate the ability of this antagonist to colonize the orange surface. Copyright © 2014 Elsevier B.V. All rights reserved.

Advances in understanding the surface chemistry of lignocellulosic biomass via time-of-flight secondary ion mass spectrometry

DOE PAGES

Tolbert, Allison K.; Ragauskas, Arthur J.

2016-12-12

Overcoming the natural recalcitrance of lignocellulosic biomass is necessary in order to efficiently convert biomass into biofuels or biomaterials and many times this requires some type of chemical pretreatment and/or biological treatment. While bulk chemical analysis is the traditional method of determining the impact a treatment has on biomass, the chemistry on the surface of the sample can differ from the bulk chemistry. Specifically, enzymes and microorganisms bind to the surface of the biomass and their efficiency could be greatly impacted by the chemistry of the surface. Therefore, it is important to study and understand the chemistry of the biomassmore » at the surface. Time-of- flight secondary ion mass spectrometry (ToF-SIMS) is a powerful tool that can spectrally and spatially analyze the surface chemistry of a sample. This review discusses the advances in understanding lignocellulosic biomass surface chemistry using the ToF-SIMS by addressing the instrument parameters, biomass sample preparation, and characteristic lignocellulosic ion fragmentation peaks along with their typical location in the plant cell wall. Furthermore, the use of the ToF-SIMS in detecting chemical changes due to chemical pretreatments, microbial treatments, and physical or genetic modifications is discussed along with possible future applications of the instrument in lignocellulosic biomass studies.« less

Advances in understanding the surface chemistry of lignocellulosic biomass via time-of-flight secondary ion mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tolbert, Allison K.; Ragauskas, Arthur J.

Overcoming the natural recalcitrance of lignocellulosic biomass is necessary in order to efficiently convert biomass into biofuels or biomaterials and many times this requires some type of chemical pretreatment and/or biological treatment. While bulk chemical analysis is the traditional method of determining the impact a treatment has on biomass, the chemistry on the surface of the sample can differ from the bulk chemistry. Specifically, enzymes and microorganisms bind to the surface of the biomass and their efficiency could be greatly impacted by the chemistry of the surface. Therefore, it is important to study and understand the chemistry of the biomassmore » at the surface. Time-of- flight secondary ion mass spectrometry (ToF-SIMS) is a powerful tool that can spectrally and spatially analyze the surface chemistry of a sample. This review discusses the advances in understanding lignocellulosic biomass surface chemistry using the ToF-SIMS by addressing the instrument parameters, biomass sample preparation, and characteristic lignocellulosic ion fragmentation peaks along with their typical location in the plant cell wall. Furthermore, the use of the ToF-SIMS in detecting chemical changes due to chemical pretreatments, microbial treatments, and physical or genetic modifications is discussed along with possible future applications of the instrument in lignocellulosic biomass studies.« less

An analytical approach to Sr isotope ratio determination in Lambrusco wines for geographical traceability purposes.

PubMed

Durante, Caterina; Baschieri, Carlo; Bertacchini, Lucia; Bertelli, Davide; Cocchi, Marina; Marchetti, Andrea; Manzini, Daniela; Papotti, Giulia; Sighinolfi, Simona

2015-04-15

Geographical origin and authenticity of food are topics of interest for both consumers and producers. Among the different indicators used for traceability studies, (87)Sr/(86)Sr isotopic ratio has provided excellent results. In this study, two analytical approaches for wine sample pre-treatment, microwave and low temperature mineralisation, were investigated to develop accurate and precise analytical method for (87)Sr/(86)Sr determination. The two procedures led to comparable results (paired t-test, with t

Short-time pretreatment of wood with low-concentration and room-temperature ionic liquid for SEM observation.

PubMed

Yamashita, Taiji; Miyamoto, Kenji; Yonenobu, Hitoshi

2018-06-20

A new pretreatment method using room-temperature ionic liquid (IL) was proposed for observing wood specimens in scanning electron microscopy (SEM). A variety of concentrations were examined for ethanol solution of the IL, [Emim][MePO3Me], to determine an optimal pretreatment procedure. It was concluded that 10% ethanol solution of the IL was the most adequate to acquire good SEM images. Using the procedure optimized, SEM images were taken for typical anatomical types of modern soft and hardwood species and archeological wood. SEM images taken were sufficiently good in observing wood cells. The pretreatment method was also effective to archeological wood dated ca. 1600 years ago. It was thus concluded that the method developed in this study is more useful than those conventionally used. Additionally, pretreatment at the high temperature was performed to confirm morphological changes in softwood. Deformation of latewood cells (tracheids) was occurred by treating with undiluted IL at the high temperature of 50°C, probably due to higher accessibility of the IL into intercellular space. Nonetheless, it was confirmed that this happens under far more extreme conditions than our proposed method.

Fast procedure for the analysis of poly(hydroxyalkanoates) in bacterial cells by off-line pyrolysis/gas-chromatography with flame ionization detector.

PubMed

Torri, Cristian; Cordiani, Helena; Samorì, Chiara; Favaro, Lorenzo; Fabbri, Daniele

2014-09-12

Poly(hydroxyalkanoates) (PHAs) are polyesters formed by saturated short chain hydroxyacids, among which 3-hydroxybutanoic (HB) and 3-hydroxypentanoic (3-hydroxyvalerate, HV) are the most common monomers of homopolymers (e.g. poly(3-hydroxybutyrate), PHB) and copolymers (e.g. poly(3-hydroxybutyrate-co-3-hydroxyhexanoate), PHB-HC). The most widely used approach for their determination is the polymer methanolysis followed by gas chromatography-mass spectrometry (GC-MS) analysis of the methylated monomers; this procedure generally requires the use of additional reagents (e.g. sulfuric acid) and is performed with harmful chlorinated solvents, such as chloroform. The development of fast routine solventless methods for the quantitative determination of PHAs and their monomeric composition is highly desirable to reduce sample pretreatment, speed up the analysis and decrease overall costs. It has been reported that under thermal treatment (e.g. pyrolysis, Py), PHAs are degraded in high yield (>40%, w/wPHA) into the corresponding 2-alkenoic acid (e.g. crotonic acid from PHB). This work aimed at investigating this reaction for direct analysis of PHAs in bacterial cells. The sample was directly subjected to pyrolysis and trapped pyrolysis products were analyzed by GC-FID. Off-line Py/GC-FID was first optimized on pure polymers with different monomer composition (PHB, PHB-HV, PHB-HC) and then applied to bacterial samples deriving from both mixed microbial cultures or selected strains, containing various types and amounts of PHAs. The Py/GC-FID method provided RSD <15% range, limit of detection of 100μg (1% PHAs in biomass), and results comparable to that of methanolysis (R(2)=0.9855), but with minimal sample pretreatment. Copyright © 2014 Elsevier B.V. All rights reserved.

Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples.

PubMed

Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Zhu, Gang-Tian; Yuan, Bi-Feng; Feng, Yu-Qi

2016-01-01

In this study, we proposed a method to fabricate magnetic carbon nitride (CN) nanosheets by simple physical blending. Low-cost CN nanosheets prepared by urea possessed a highly π-conjugated structure; therefore the obtained composites were employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oil samples. Moreover, sample pre-treatment time could be carried out within 10 min. Thus, a simple and cheap method for the analysis of PAHs in edible oil samples was established by coupling magnetic CN nanosheets-based MSPE with gas chromatography-mass spectrometry (GC/MS) analysis. Limits of quantitation (LOQs) for eight PAHs ranged from 0.4 to 0.9 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 15.0%. The recoveries of PAHs for spiked soybean oil samples ranged from 91.0% to 124.1%, with RSDs of less than 10.2%. Taken together, the proposed method offers a simple and cost-effective option for the convenient analysis of PAHs in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimization of solid-phase extraction and liquid chromatography-tandem mass spectrometry for simultaneous determination of capilliposide B and its active metabolite in rat urine and feces: Overcoming nonspecific binding.

PubMed

Cheng, Zhongzhe; Zhou, Xing; Li, Wenyi; Hu, Bingying; Zhang, Yang; Xu, Yong; Zhang, Lin; Jiang, Hongliang

2016-11-30

Capilliposide B, a novel oleanane triterpenoid saponin isolated from Lysimachia capillipes Hemsl, showed significant anti-tumor activities in recent studies. To characterize the excretion of Capilliposide B, a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of Capilliposide B and its active metabolite, Capilliposide A in rat urine and feces. Sample preparation using a solid-phase extraction procedure was optimized by acidification of samples at various degrees, providing extensive sample clean-up with a high extraction recovery. In addition, rat urinary samples were pretreated with CHAPS, an anti-adsorptive agent, for overcoming nonspecific analytes adsorption during sample storage and process. The method validation was conducted over the curve range of 10.0-5000ng/ml for both analytes. The intra- and inter-day precision and accuracy of the QC samples showed ≤11.0% RSD and -10.4-12.8% relative error. The method was successfully applied to an excretion study of Capilliposide B following intravenous administration. Copyright © 2016 Elsevier B.V. All rights reserved.

Pre-Treatment Objective Diagnosis and Post-Treatment Outcome Evaluation in Patients with Vascular Pulsatile Tinnitus Using Transcanal Recording and Spectro-Temporal Analysis

PubMed Central

Choi, Inyong; Koo, Ja-Won; Lee, Kyogu

2016-01-01

Objective Although vascular pulsatile tinnitus (VPT) has been classified as “objective”, VPT is not easily recognizable or documentable in most cases. In response to this, we have developed transcanal sound recording (TSR) and spectro-temporal analysis (STA) for the objective diagnosis of VPT. By refining our initial method, we were able to apply TSR/STA to post-treatment outcome evaluation, as well as pre-treatment objective diagnosis. Methods TSR was performed on seven VPT patients and five normal controls before and after surgical or interventional treatment. VPT was recorded using an inserted microphone with the subjects placed in both upright and supine positions with 1) a neutral head position, 2) head rotated to the tinnitus side, 3) head rotated to the non-tinnitus side, and 4) a neutral position with ipsi-lesional manual cervical compression. The recorded signals were analyzed in both time and time-frequency domains by performing a short-time Fourier transformation. Results The pre-treatment ear canal signals of all VPT patients demonstrated pulse-synchronous periodic structures and acoustic characteristics that were representative of their presumptive vascular pathologies, whereas those the controls exhibited smaller peaks and weak periodicities. Compared with the pre-treatment signals, the post-treatment signals exhibited significantly reduced peak- and root mean square amplitudes upon time domain analysis. Additionally, further sub-band analysis confirmed that the pulse-synchronous signal of all subjects was not identifiable after treatment and, in particular, that the signal decrement was statistically significant at low frequencies. Moreover, the post-treatment signals of the VPT subjects revealed no significant differences when compared to those of the control group. Conclusion We reconfirmed that the TSR/STA method is an effective modality to objectify VPT. In addition, the potential role of the TSR/STA method in the objective evaluation of treatment outcomes in patients with VPT was proven. Further studies incorporating a larger sample size and more refined recording techniques are warranted. PMID:27351198

Determination of somatropin charged variants by capillary zone electrophoresis - optimisation, verification and implementation of the European pharmacopoeia method.

PubMed

Storms, S M; Feltus, A; Barker, A R; Joly, M-A; Girard, M

2009-03-01

Measurement of somatropin charged variants by isoelectric focusing was replaced with capillary zone electrophoresis in the January 2006 European Pharmacopoeia Supplement 5.3, based on results from an interlaboratory collaborative study. Due to incompatibilities and method-robustness issues encountered prior to verification, a number of method parameters required optimisation. As the use of a diode array detector at 195 nm or 200 nm led to a loss of resolution, a variable wavelength detector using a 200 nm filter was employed. Improved injection repeatability was obtained by increasing the injection time and pressure, and changing the sample diluent from water to running buffer. Finally, definition of capillary pre-treatment and rinse procedures resulted in more consistent separations over time. Method verification data are presented demonstrating linearity, specificity, repeatability, intermediate precision, limit of quantitation, sample stability, solution stability, and robustness. Based on these experiments, several modifications to the current method have been recommended and incorporated into the European Pharmacopoeia to help improve method performance across laboratories globally.

Improvement of organoleptic quality of retted cassava products by alkali pretreatment of roots and addition of sodium nitrate during retting.

PubMed

Ogbo, Frank C

2003-12-15

Alkali pretreatment of cassava roots before retting and addition of sodium nitrate during retting were used to manipulate the metabolism of microorganisms involved in cassava (Manihot esculenta Crantz) retting, as a method for removing the characteristic offensive odour of retted cassava products. Odour was assessed by organoleptic methods. The characteristics of fermentation of cassava by the traditional method (control) were as follows; aerobic mesophilic count (APC) on nutrient agar (NA) at 30 degrees C/48 h, attained a maximum of 2.3 x 10(7)/ml retting juice while counts on de Man Rogosa and Sharpe agar (MRS) at 30 degrees C/48 h were 1.6 x 10(8)/ml. Maximum titrable acidity was 0.062% lactic acid by weight of retting juice. Cassava was retted in 3 days and the product exhibited characteristic offensive odour. Addition of NaNO3 into retting water effectively removed odour at a concentration of 0.3 g/l. Maximum APC on NA/30 degrees C/48 h was 6.8 x 10(6)/ml. Counts on MRS/30 degrees C/48 h exceeded 2.4 x 10(9)/ml. Retting was complete in 3 days with a final titrable acidity of 0.068% of retting juice. Removal of odour likely resulted from selection of homo-fermentative lactic acid bacteria, thus producing mostly odourless lactic acid. Alkali pretreatment of roots before retting was efficacious in removing odour at a concentration of 10 g/l for 30 min. This fermentation was characterized by APC on NA/30 degrees C/48 h of 5.4 x 10(6)/ml; MRS/30 degrees C/48 h reached a maximum of only 10 x 10(4)/ml and correspondingly low titrable acidity of 0.003%. Low counts of lactic acid bacteria correlate well with the absence of odour in this sample. Both treatments did not adversely affect the detoxification process, yielding "foo-foo" with HCN levels lower than 10 mg/kg. Residual nitrates and nitrites of 30 mg/kg in the sodium nitrate-treated sample were also within the safe limits of 156 mg/kg allowed in many countries. Organoleptically improved samples were acceptable to the public.

Hexavalent Chrome Free Coatings for Electronics: Electromagnetic Interference (EMI) Shielding Effectiveness (SE)

NASA Technical Reports Server (NTRS)

Kessel, Kurt R.

2016-01-01

Determine the suitability of trivalent chromium conversion coatings that meet the requirements of MIL-DTL-5541, Type II, for use in applications where high-frequency electrical performance is important. Evaluate the ability of hexavalent chrome free pretreated aluminum to form adequate EMI seals, and maintain that seal while being subjected to harsh environmental conditions. Assess the performance of trivalent chromium pretreatments against a known control hexavalent chrome pretreatment before and after they have been exposed to a set of environmental conditions. It is known that environmental testing causes a decrease in shielding effectiveness when hexavalent chrome pretreatments are used (Alodine 1200s). Need to determine how shielding effectiveness will be affected with the use of hexavalent chrome free pretreatments. Performance will be assessed by evaluating shielding effectiveness (SE) test data from a variety of test samples comprised of different aluminum types and/or conversion coatings. The formation of corrosion will be evaluated between the mating surfaces and gasket to assess the corrosion resistant properties of the pretreatments, comparing the hexavalent control to the hexavalent chrome free pretreatments.

[Fast discrimination of edible vegetable oil based on Raman spectroscopy].

PubMed

Zhou, Xiu-Jun; Dai, Lian-Kui; Li, Sheng

2012-07-01

A novel method to fast discriminate edible vegetable oils by Raman spectroscopy is presented. The training set is composed of different edible vegetable oils with known classes. Based on their original Raman spectra, baseline correction and normalization were applied to obtain standard spectra. Two characteristic peaks describing the unsaturated degree of vegetable oil were selected as feature vectors; then the centers of all classes were calculated. For an edible vegetable oil with unknown class, the same pretreatment and feature extraction methods were used. The Euclidian distances between the feature vector of the unknown sample and the center of each class were calculated, and the class of the unknown sample was finally determined by the minimum distance. For 43 edible vegetable oil samples from seven different classes, experimental results show that the clustering effect of each class was more obvious and the class distance was much larger with the new feature extraction method compared with PCA. The above classification model can be applied to discriminate unknown edible vegetable oils rapidly and accurately.

Quantitative determination of total cesium in highly active liquid waste by using liquid electrode plasma optical emission spectrometry.

PubMed

Do, Van-Khoai; Yamamoto, Masahiko; Taguchi, Shigeo; Takamura, Yuzuru; Surugaya, Naoki; Kuno, Takehiko

2018-06-01

A sensitive analytical method for determination of total cesium (Cs) in highly active liquid waste (HALW) by using modified liquid electrode plasma optical emission spectrometry (LEP-OES) is developed in this study. The instrument is modified to measure radioactive samples in a glove box. The effects of important factors, including pulsed voltage sequence and nitric acid concentration, on the emission of Cs are investigated. The limit of detection (LOD) and limit of quantification (LOQ) are 0.005 mg/L and 0.02 mg/L, respectively. The achieved LOD is one order lower than that of recently developed spectroscopic methods using liquid discharge plasma. The developed method is validated by subjecting a simulated HALW sample to inductively coupled plasma mass spectrometry (ICP-MS). The recoveries obtained from a spike-and-recovery test are 96-102%, implying good accuracy. The method is successfully applied to the quantification of Cs in a real HALW sample at the Tokai reprocessing plant in Japan. Apart from dilution and filtration of the HALW sample, no other pre-treatment process is required. The results agree well with the values obtained using gamma spectrometry. The developed method offers a reliable technique for rapid analysis of total Cs in HALW samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Construction and field test of a programmable and self-cleaning auto-sampler controlled by a low-cost one-board computer

NASA Astrophysics Data System (ADS)

Stadler, Philipp; Farnleitner, Andreas H.; Zessner, Matthias

2016-04-01

This presentation describes in-depth how a low cost micro-computer was used for substantial improvement of established measuring systems due to the construction and implementation of a purposeful complementary device for on-site sample pretreatment. A fully automated on-site device was developed and field-tested, that enables water sampling with simultaneous filtration as well as effective cleaning procedure of the devicés components. The described auto-sampler is controlled by a low-cost one-board computer and designed for sample pre-treatment, with minimal sample alteration, to meet requirements of on-site measurement devices that cannot handle coarse suspended solids within the measurement procedure or -cycle. The automated sample pretreatment was tested for over one year for rapid and on-site enzymatic activity (beta-D-glucuronidase, GLUC) determination in sediment laden stream water. The formerly used proprietary sampling set-up was assumed to lead to a significant damping of the measurement signal due to its susceptibility to clogging, debris- and bio film accumulation. Results show that the installation of the developed apparatus considerably enhanced error-free running time of connected measurement devices and increased the measurement accuracy to an up-to-now unmatched quality.

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate.

PubMed

Lee, S C; Zou, S C; Ho, K F; Chan, L Y

2001-01-02

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25-50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption (100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.

Ultrahigh-Performance Liquid Chromatography (UHPLC)-Tandem Mass Spectrometry (MS/MS) Quantification of Nine Target Indoles in Sparkling Wines.

PubMed

Tudela, Rebeca; Ribas-Agustí, Albert; Buxaderas, Susana; Riu-Aumatell, Montserrat; Castellari, Massimo; López-Tamames, Elvira

2016-06-15

An ultrahigh-performance liquid chromatography (UHPLC)-tandem mass spectrometry (MS/MS) method was developed for the simultaneous determination of nine target indoles in sparkling wines. The proposed method requires minimal sample pretreatment, and its performance parameters (accuracy, repeatability, LOD, and matrix effect) indicate that it is suitable for routine analysis. Four indoles were found at detectable levels in commercial Cava samples: 5-methoxytryptophol (5MTL), tryptophan (TRP), tryptophan ethyl ester (TEE), and N-acetylserotonin (NSER). Two of them, NSER and 5MTL, are reported here for the first time in sparkling wines, with values of 0.3-2 and 0.29-29.2 μg/L, respectively. In the same samples, the contents of melatonin (MEL), serotonin (SER), 5-hydroxytryptophan (5-OHTRP), 5-hydroxyindole-3-acetic acid (5OHIA), and 5-methoxy-3-indoleacetic acid (5MIA) were all below the corresponding limits of detection.

Utilizing pretreatment and fungal incubation to enhance the nutritional value of canola meal

USDA-ARS?s Scientific Manuscript database

The objective of this study was to determine the optimal pretreatment and fungal strain to reduce glucosinolates (GLS), fiber, and residual sugars while increasing the nutritional value of canola meal. Submerged incubation conditions were used to evaluate four pretreatment methods (extrusion, hot wa...

Biological pretreatment of corn stover with white-rot fungus for enzymatic hydrolysis and bioethanol production

USDA-ARS?s Scientific Manuscript database

Pretreatment, as the first step towards conversion of lignocellulosic feedstocks to biofuels and/or chemicals remains one of the main barriers to commercial success. Typically, harsh methods are used to pretreat lignocellulosic biomass prior to its breakdown to sugars by enzymes, which also result ...

Pre-treatment for molybdenum or molybdenum-rich alloy articles to be plated

DOEpatents

Wright, Ralph R.

1980-01-01

This invention is a method for etching a molybdenum or molybdenum-rich alloy surface to promote the formation of an adherent bond with a subsequently deposited metallic plating. In a typical application, the method is used as a pre-treatment for surfaces to be electrolessly plated with nickel. The pre-treatment comprises exposing the crystal boundaries of the surface by (a) anodizing the surface in acidic solution to form a continuous film of gray molybdenum oxide thereon and (b) removing the film.

Optimizing Phosphoric Acid plus Hydrogen Peroxide (PHP) Pretreatment on Wheat Straw by Response Surface Method for Enzymatic Saccharification.

PubMed

Qiu, Jingwen; Wang, Qing; Shen, Fei; Yang, Gang; Zhang, Yanzong; Deng, Shihuai; Zhang, Jing; Zeng, Yongmei; Song, Chun

2017-03-01

Wheat straw was pretreated by phosphoric acid plus hydrogen peroxide (PHP), in which temperature, time, and H 3 PO 4 proportion for pretreatment were investigated by using response surface method. Results indicated that hemicellulose and lignin removal positively responded to the increase of pretreatment temperature, H 3 PO 4 proportion, and time. H 3 PO 4 proportion was the most important variable to control cellulose recovery, followed by pretreatment temperature and time. Moreover, these three variables all negatively related to cellulose recovery. Increasing H 3 PO 4 proportion can improve enzymatic hydrolysis; however, reduction on cellulose recovery results in decrease of glucose yield. Extra high temperature or long time for pretreatment was not beneficial to enzymatic hydrolysis and glucose yield. Based on the criterion for minimizing H 3 PO 4 usage and maximizing glucose yield, the optimized pretreatment conditions was 40 °C, 2.0 h, and H 3 PO 4 proportion of 70.2 % (H 2 O 2 proportion of 5.2 %), by which glucose yielded 299 mg/g wheat straw (946.2 mg/g cellulose) after 72-h enzymatic hydrolysis.

Physical Pretreatment Methods for Improving Microalgae Anaerobic Biodegradability.

PubMed

Córdova, Olivia; Passos, Fabiana; Chamy, Rolando

2018-05-01

Microalgae may be a potential feedstock for biogas production through anaerobic digestion. However, this process is limited by the hydrolytic stage, due to the complex and resistant microalgae cell wall components. This fact hinders biomass conversion into biogas, demanding the application of pretreatment techniques for inducing cell damage and/or lysis and organic matter solubilisation. In this study, sonication, thermal, ultrasound, homogeneizer, hydrothermal and steam explosion pretreatments were evaluated in different conditions for comparing their effects on anaerobic digestion performance in batch reactors. The results showed that the highest biomass solubilisation values were reached for steam explosion (65-73%) and ultrasound (33-57%). In fact, only applied energies higher than 220 W or temperatures higher than 80 °C induced cell wall lysis in C. sorokiniana. Nonetheless, the highest methane yields were not correlated to biogas production. Thermal hydrolysis and steam explosion showed lower methane yields in respect to non-pretreated biomass, suggesting the presence of toxic compounds that inhibited the biological process. Accordingly, these pretreatment techniques led to a negative energy balance. The best pretreatment method among the ones evaluated was thermal pretreatment, with four times more energy produced that demanded.

Treatment Attrition: Associations with Negative Affect Smoking Motives and Barriers to Quitting Among Treatment-Seeking Smokers

PubMed Central

Garey, Lorra; Kauffman, Brooke Y.; Neighbors, Clayton; Schmidt, Norman B.; Zvolensky, Michael J.

2016-01-01

Introduction Pre-treatment attrition and perceived barriers for quitting are clinically important processes involved in early phases of quitting smoking. However, less is known about the constructs that may contribute to these processes such as negative affect reduction smoking motives. Method The current study sought to evaluate the relation between negative affect reduction smoking motives with pre-treatment attrition and perceived barriers for quitting in a sample of 425 treatment-seeking smokers (48.5% female; Mage = 37.69; SD = 13.61) enrolled in a smoking cessation study examining the efficacy of a transdiagnostic panic-smoking cessation treatment relative to a standard smoking cessation treatment. Results Results indicated that greater negative affect reduction smoking motives was associated with an increased likelihood of treatment initiation (Odds Ratio = 1.49, CI: 1.09, 2.04). Additionally, negative affect reduction smoking motives was associated with greater perceived barriers for cessation among pre-treatment drop-outs and treatment initiators. Conclusions This initial investigation provides evidence for the possible clinical utility in addressing negative affect reduction smoking motives during early stages of quitting. Additionally, such findings could potentially inform the development of personalized, early stages of quitting interventions for smoking cessation. PMID:27518764

Automation of ⁹⁹Tc extraction by LOV prior ICP-MS detection: application to environmental samples.

PubMed

Rodríguez, Rogelio; Leal, Luz; Miranda, Silvia; Ferrer, Laura; Avivar, Jessica; García, Ariel; Cerdà, Víctor

2015-02-01

A new, fast, automated and inexpensive sample pre-treatment method for (99)Tc determination by inductively coupled plasma-mass spectrometry (ICP-MS) detection is presented. The miniaturized approach is based on a lab-on-valve (LOV) system, allowing automatic separation and preconcentration of (99)Tc. Selectivity is provided by the solid phase extraction system used (TEVA resin) which retains selectively pertechnetate ion in diluted nitric acid solution. The proposed system has some advantages such as minimization of sample handling, reduction of reagents volume, improvement of intermediate precision and sample throughput, offering a significant decrease of both time and cost per analysis in comparison to other flow techniques and batch methods. The proposed LOV system has been successfully applied to different samples of environmental interest (water and soil) with satisfactory recoveries, between 94% and 98%. The detection limit (LOD) of the developed method is 0.005 ng. The high durability of the resin and its low amount (32 mg), its good intermediate precision (RSD 3.8%) and repeatability (RSD 2%) and its high extraction frequency (up to 5 h(-1)) makes this method an inexpensive, high precision and fast tool for monitoring (99)Tc in environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

2016-04-01

High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple micro-photometric method for urinary iodine determination.

PubMed

Grimm, Gabriele; Lindorfer, Heidelinde; Kieweg, Heidi; Marculescu, Rodrig; Hoffmann, Martha; Gessl, Alois; Sager, Manfred; Bieglmayer, Christian

2011-10-01

Urinary iodide concentration (UIC) is useful to evaluate nutritional iodine status. In clinical settings UIC helps to exclude blocking of the thyroid gland by excessive endogenous iodine, if diagnostic or therapeutic administration of radio-iodine is indicated. Therefore, this study established a simple test for the measurement of UIC. UIC was analyzed in urine samples of 200 patients. Samples were pre-treated at 95°C for 45 min with ammonium persulfate in a thermal cycler, followed by a photometric Sandell-Kolthoff reaction (SK) carried out in microtiter plates. For method comparison, UIC was analyzed in 30 samples by inductivity coupled plasma mass spectro-metry (ICP-MS) as a reference method. Incubation conditions were optimized concerning recovery. The photometric test correlated well to the reference method (SK=0.91*ICP-MS+1, r=0.962) and presented with a functional sensitivity of 20 μg/L. UIC of patient samples ranged from <20 to 750 μg/L (median 110 μg/L); 90% of the urine samples had iodide concentrations below 210 μg/L. The modified SK-test takes approximately 90 min for analyses of 20 urine samples compared with 27 h for ICP-MS. The photometric test provides satisfactory results and can be performed with the basic equipment of a clinical laboratory.

Application of Magnetic Nanoparticles in Pretreatment Device for POPs Analysis in Water

NASA Astrophysics Data System (ADS)

Chu, Dongzhi; Kong, Xiangfeng; Wu, Bingwei; Fan, Pingping; Cao, Xuan; Zhang, Ting

2018-01-01

In order to reduce process time and labour force of POPs pretreatment, and solve the problem that extraction column was easily clogged, the paper proposed a new technology of extraction and enrichment which used magnetic nanoparticles. Automatic pretreatment system had automatic sampling unit, extraction enrichment unit and elution enrichment unit. The paper briefly introduced the preparation technology of magnetic nanoparticles, and detailly introduced the structure and control system of automatic pretreatment system. The result of magnetic nanoparticles mass recovery experiments showed that the system had POPs analysis preprocessing capability, and the recovery rate of magnetic nanoparticles were over 70%. In conclusion, the author proposed three points optimization recommendation.

Adequacy of laser diffraction for soil particle size analysis

PubMed Central

Fisher, Peter; Aumann, Colin; Chia, Kohleth; O'Halloran, Nick; Chandra, Subhash

2017-01-01

Sedimentation has been a standard methodology for particle size analysis since the early 1900s. In recent years laser diffraction is beginning to replace sedimentation as the prefered technique in some industries, such as marine sediment analysis. However, for the particle size analysis of soils, which have a diverse range of both particle size and shape, laser diffraction still requires evaluation of its reliability. In this study, the sedimentation based sieve plummet balance method and the laser diffraction method were used to measure the particle size distribution of 22 soil samples representing four contrasting Australian Soil Orders. Initially, a precise wet riffling methodology was developed capable of obtaining representative samples within the recommended obscuration range for laser diffraction. It was found that repeatable results were obtained even if measurements were made at the extreme ends of the manufacturer’s recommended obscuration range. Results from statistical analysis suggested that the use of sample pretreatment to remove soil organic carbon (and possible traces of calcium-carbonate content) made minor differences to the laser diffraction particle size distributions compared to no pretreatment. These differences were found to be marginally statistically significant in the Podosol topsoil and Vertosol subsoil. There are well known reasons why sedimentation methods may be considered to ‘overestimate’ plate-like clay particles, while laser diffraction will ‘underestimate’ the proportion of clay particles. In this study we used Lin’s concordance correlation coefficient to determine the equivalence of laser diffraction and sieve plummet balance results. The results suggested that the laser diffraction equivalent thresholds corresponding to the sieve plummet balance cumulative particle sizes of < 2 μm, < 20 μm, and < 200 μm, were < 9 μm, < 26 μm, < 275 μm respectively. The many advantages of laser diffraction for soil particle size analysis, and the empirical results of this study, suggest that deployment of laser diffraction as a standard test procedure can provide reliable results, provided consistent sample preparation is used. PMID:28472043

Combination of alkaline and microwave pretreatment for disintegration of meat processing wastewater sludge.

PubMed

Erden, G

2013-01-01

Meat processing wastewater sludge has high organic content but it is very slow to degrade in biological processes. Anaerobic digestion may be a good alternative for this type of sludge when the hydrolysis, known to be the rate-limiting step of biological sludge anaerobic degradation, could be eliminated by disintegration. This investigation deals with disintegration of meat processing wastewater sludge. Microwave (MW) irradiation and combined alkaline pretreatment and MW irradiation were applied to sludge for disintegration purposes. Disintegration performance of the methods was evaluated with disintegration degree based on total and dissolved organic carbon calculations (DD(TOC)), and the solubilization of volatile solids (S(VS)) in the pretreated sludge. Optimum conditions were found to be 140 degrees C and 30 min for MW irradiation using response surface methodology (RSM) and pH = 13 for combined pretreatment. While DD(TOC) was observed as 24.6% and 54.9, S(VS) was determined as 8.54% and 42.5% for MW pretreated and combined pretreated sludge, respectively. The results clearly show that pre-conditioning of sludge with alkaline pretreatment played an important role in enhancing the disintegration efficiency of subsequent MW irradiation. Disintegration methods also affected the anaerobic biodegradability and dewaterability of sludge. An increase of 23.6% in biogas production in MW irradiated sludge was obtained, comparing to the raw sludge at the end of the 35 days of incubation. This increase was observed as 44.5% combined pretreatment application. While MW pretreatment led to a little improvement of the dewatering performance of sludge, in combined pretreatment NaOH deteriorates the sludge dewaterability.

Pretreatment of corn stover using low-moisture anhydrous ammonia (LMAA) process.

PubMed

Yoo, Chang Geun; Nghiem, Nhuan P; Hicks, Kevin B; Kim, Tae Hyun

2011-11-01

A simple pretreatment method using anhydrous ammonia was developed to minimize water and ammonia inputs for cellulosic ethanol production, termed the low moisture anhydrous ammonia (LMAA) pretreatment. In this method, corn stover with 30-70% moisture was contacted with anhydrous ammonia in a reactor under nearly ambient conditions. After the ammoniation step, biomass was subjected to a simple pretreatment step at moderate temperatures (40-120°C) for 48-144 h. Pretreated biomass was saccharified and fermented without an additional washing step. With 3% glucan loading of LMAA-treated corn stover under best treatment conditions (0.1g-ammonia+1.0 g-water per g biomass, 80°C, and 84 h), simultaneous saccharification and cofermentation test resulted in 24.9 g/l (89% of theoretical ethanol yield based on glucan+xylan in corn stover). Copyright © 2011 Elsevier Ltd. All rights reserved.

Microalgal lipid production using the hydrolysates of rice straw pretreated with gamma irradiation and alkali solution.

PubMed

Joe, Min-Ho; Kim, Ji-Youn; Lim, Sangyong; Kim, Dong-Ho; Bai, Suk; Park, Hyun; Lee, Sung Gu; Han, Se Jong; Choi, Jong-Il

2015-01-01

Lignocellulosic biomass has long been recognized as a potential sustainable source of sugars for biofuels. However, many physicochemical structural and compositional factors inhibit the enzymatic digestibility of the lignocellulosic biomass. In this study, efficient pretreatment method of rice straw (RS) was developed and the RS hydrolysate was applied in the cultivation of microalgae for lipid production. Gamma ray irradiation (GRI) and alkali solution were used for the pretreatment, and saccharification was carried out with lignocellulolytic enzymes. When RS was pretreated by combined GRI and alkali method, the glucose and xylose saccharification yield after enzymatic hydrolysis increased up to 91.65 and 98.84 %, respectively. The enzymatic hydrolysate from the RS pretreated with the combined method was used to cultivate Chlorella protothecoides for lipid production. The maximum concentrations of biomass and fatty acid methyl ester of cells were 6.51 and 2.95 g/L, respectively. The lipid content of C. protothecoides from RS hydrolysate was comparable to that from glucose, and the lipid composition was similar between different carbon sources. These results demonstrate that the combined pretreatment with gamma irradiation was highly effective in preparing hydrolysate, and the rice straw hydrolysate could be used as an alternative carbon source for microalgal lipid production for biofuel.

Effects of water washing and torrefaction pretreatments on rice husk pyrolysis by microwave heating.

PubMed

Zhang, Shuping; Dong, Qing; Zhang, Li; Xiong, Yuanquan; Liu, Xinzhi; Zhu, Shuguang

2015-10-01

The influences of water washing, torrefaction and combined water washing-torrefaction pretreatments on microwave pyrolysis of rice husk samples were investigated. The results indicated that the process of combined water washing-torrefaction pretreatment could effectively remove a large portion of inorganics and improve the fuel characteristics to a certain extent. The gas products were rich in combustible compositions and the syngas quality was improved by pretreatment process. The liquid products contained less moisture content, acids and furans, while more concentrated phenols and sugars from microwave pyrolysis of rice husk after pretreatments, especially after the combined water washing-torrefaction pretreatment. Biochar, produced in high yield, has the alkaline pH (pH 8.2-10.0) and high surface area (S(BET) 157.81-267.84 m(2)/g), they have the potential to be used as soil amendments. It is noteworthy that water washing increased the pore surface area of biochar, but torrefaction reduced the pore surface area. Copyright © 2015 Elsevier Ltd. All rights reserved.

Biomethane production and physicochemical characterization of anaerobically digested teff (Eragrostis tef) straw pretreated by sodium hydroxide.

PubMed

Chufo, Akiber; Yuan, Hairong; Zou, Dexun; Pang, Yunzhi; Li, Xiujin

2015-04-01

The biogas production potential and biomethane content of teff straw through pretreatment by NaOH was investigated. Different NaOH concentrations (1%, 2%, 4% and 6%) were used for each four solid loadings (50, 65, 80 and 95 g/L). The effects of NaOH as pretreatment factor on the biodegradability of teff straw, changes in main compositions and enhancement of anaerobic digestion were analyzed. The result showed that, using 4% NaOH for pretreatment in 80 g/L solid loading produced 40.0% higher total biogas production and 48.1% higher biomethane content than the untreated sample of teff straw. Investigation of changes in chemical compositions and physical microstructure indicated that there was 4.3-22.1% total lignocellulosic compositions removal after three days pretreatment with NaOH. The results further revealed that NaOH pretreatment changed the structural compositions and lignin network, and improved biogas production from teff straw. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microwave-assisted acid pretreatment of alkali lignin: Effect on characteristics and pyrolysis behavior.

PubMed

Duan, Dengle; Ruan, Roger; Wang, Yunpu; Liu, Yuhuan; Dai, Leilei; Zhao, Yunfeng; Zhou, Yue; Wu, Qiuhao

2018-03-01

This study performed microwave-assisted acid pretreatment on pure lignin. The effects of microwave temperature, microwave time, and hydrochloric acid concentration on characteristics and pyrolysis behavior of lignin were examined. Results of ultimate analysis revealed better properties of all pretreated samples than those of raw lignin. Fourier transform infrared spectroscopy analysis showed breakage of βO4 bond and aliphatic side chain, decrease in OH groups, and formation of CO groups in pretreatment. Microwave temperature exerted more significant influence on lignin structure. Thermal stability of treated lignin was improved and insensitive to short microwave time and acid concentration under mild conditions. Resulting from improved alkyl-phenols and decreased alkoxy-phenols, microwave-assisted acid pretreatment of lignin yielded bio-oil with excellent quality. Total yield of phenols in pyrolysis vapors (200 °C) improved to 14.15%, whereas that of guaiacols decreased to 22.36%. This study shows that microwave-assisted acid pretreatment is a promising technology for lignin conversion. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evaluation of propidium monoazide (PMA) treatment directly on membrane filter for the enumeration of viable but non cultivable Legionella by qPCR.

PubMed

Slimani, Sami; Robyns, Audrey; Jarraud, Sophie; Molmeret, Maëlle; Dusserre, Eric; Mazure, Céline; Facon, Jean Pierre; Lina, Gérard; Etienne, Jerome; Ginevra, Christophe

2012-02-01

A PMA (propidium monoazide) pretreatment protocol, in which PMA is applied directly to membrane filters, was developed for the PCR-based quantification (PMA-qPCR) of viable Legionella pneumophila. Using this method, the amplification of DNA from membrane-damaged L. pneumophila was strongly inhibited for samples containing a small number of dead bacteria. Copyright © 2011 Elsevier B.V. All rights reserved.

Effect of coagulation on treatment of municipal wastewater reverse osmosis concentrate by UVC/H2O2.

PubMed

Umar, Muhammad; Roddick, Felicity; Fan, Linhua

2014-02-15

Disposal of reverse osmosis concentrate (ROC) is a growing concern due to potential health and ecological risks. Alum coagulation was investigated as pre-treatment for the UVC/H2O2 treatment of two high salinity ROC samples (ROC A and B) of comparable organic and inorganic content. Coagulation removed a greater fraction of the organic content for ROC B (29%) than ROC A (16%) which correlated well with the reductions of colour and A254. Although the total reductions after 60 min UVC/H2O2 treatment with and without coagulation were comparable, large differences in the trends of reduction were observed which were attributed to the different nature of the organic content (humic-like) of the samples as indicated by the LC-OCD analyses and different initial (5% and 16%) biodegradability. Coagulation and UVC/H2O2 treatment preferentially removed humic-like compounds which resulted in low reaction rates after UVC/H2O2 treatment of the coagulated samples. The improvement in biodegradability was greater (2-3-fold) during UVC/H2O2 treatment of the pre-treated samples than without pre-treatment. The target DOC residual (≤ 15 mg/L) was obtained after 30 and 20 min irradiation of pre-treated ROC A and ROC B with downstream biological treatment, corresponding to reductions of 55% and 62%, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Evaluation of bank filtration as a pretreatment method for the provision of hygienically safe drinking water in Norway: results from monitoring at two full-scale sites

NASA Astrophysics Data System (ADS)

Kvitsand, Hanne M. L.; Myrmel, Mette; Fiksdal, Liv; Østerhus, Stein W.

2017-08-01

Two case studies were carried out in central Norway in order to assess the performance of bank filtration systems in cold-climate fluvial aquifers relying on recharge from humic-rich surface waters with moderate microbial contamination. Three municipal wells and two surface-water sources at operative bank filtration systems were monitored for naturally occurring bacteriophages, fecal indicators, natural organic matter (NOM) and physico-chemical water quality parameters during a 4-month period. Aquifer passage effectively reduced the microorganism and NOM concentrations at both study sites. Bacteriophages were detected in 13 of 16 (81%) surface-water samples and in 4 of 24 (17%) well-water samples, and underwent 3 ± 0.3 log10 reduction after 50-80-m filtration and 20-30 days of subsurface passage. NOM reductions (color: 74-97%; dissolved organic carbon: 54-80%; very hydrophobic acids: 70%) were similar to those achieved by conventional water-treatment processes and no further treatment was needed. Both groundwater dilution and sediment filtration contributed to the hygienic water quality improvements, but sediment filtration appeared to be the most important process with regard to microbial and NOM reductions. A strengths-weaknesses-opportunities-threats analysis showed that bank filtration technology has a high potential as a pretreatment method for the provision of hygienically safe drinking water in Norway.

Simple Elimination of Background Fluorescence in Formalin-Fixed Human Brain Tissue for Immunofluorescence Microscopy.

PubMed

Sun, Yulong; Ip, Philbert; Chakrabartty, Avijit

2017-09-03

Immunofluorescence is a common method used to visualize subcellular compartments and to determine the localization of specific proteins within a tissue sample. A great hindrance to the acquisition of high quality immunofluorescence images is endogenous autofluorescence of the tissue caused by aging pigments such as lipofuscin or by common sample preparation processes such as aldehyde fixation. This protocol describes how background fluorescence can be greatly reduced through photobleaching using white phosphor light emitting diode (LED) arrays prior to treatment with fluorescent probes. The broad-spectrum emission of white phosphor LEDs allow for bleaching of fluorophores across a range of emission peaks. The photobleaching apparatus can be constructed from off-the-shelf components at very low cost and offers an accessible alternative to commercially available chemical quenchers. A photobleaching pre-treatment of the tissue followed by conventional immunofluorescence staining generates images free of background autofluorescence. Compared to established chemical quenchers which reduced probe as well as background signals, photobleaching treatment had no effect on probe fluorescence intensity while it effectively reduced background and lipofuscin fluorescence. Although photobleaching requires more time for pre-treatment, higher intensity LED arrays may be used to reduce photobleaching time. This simple method can potentially be applied to a variety of tissues, particularly postmitotic tissues that accumulate lipofuscin such as the brain and cardiac or skeletal muscles.

Heparin removal by ecteola-cellulose pre-treatment enables the use of plasma samples for accurate measurement of anti-Yellow fever virus neutralizing antibodies.

PubMed

Campi-Azevedo, Ana Carolina; Peruhype-Magalhães, Vanessa; Coelho-Dos-Reis, Jordana Grazziela; Costa-Pereira, Christiane; Yamamura, Anna Yoshida; Lima, Sheila Maria Barbosa de; Simões, Marisol; Campos, Fernanda Magalhães Freire; de Castro Zacche Tonini, Aline; Lemos, Elenice Moreira; Brum, Ricardo Cristiano; de Noronha, Tatiana Guimarães; Freire, Marcos Silva; Maia, Maria de Lourdes Sousa; Camacho, Luiz Antônio Bastos; Rios, Maria; Chancey, Caren; Romano, Alessandro; Domingues, Carla Magda; Teixeira-Carvalho, Andréa; Martins-Filho, Olindo Assis

2017-09-01

Technological innovations in vaccinology have recently contributed to bring about novel insights for the vaccine-induced immune response. While the current protocols that use peripheral blood samples may provide abundant data, a range of distinct components of whole blood samples are required and the different anticoagulant systems employed may impair some properties of the biological sample and interfere with functional assays. Although the interference of heparin in functional assays for viral neutralizing antibodies such as the functional plaque-reduction neutralization test (PRNT), considered the gold-standard method to assess and monitor the protective immunity induced by the Yellow fever virus (YFV) vaccine, has been well characterized, the development of pre-analytical treatments is still required for the establishment of optimized protocols. The present study intended to optimize and evaluate the performance of pre-analytical treatment of heparin-collected blood samples with ecteola-cellulose (ECT) to provide accurate measurement of anti-YFV neutralizing antibodies, by PRNT. The study was designed in three steps, including: I. Problem statement; II. Pre-analytical steps; III. Analytical steps. Data confirmed the interference of heparin on PRNT reactivity in a dose-responsive fashion. Distinct sets of conditions for ECT pre-treatment were tested to optimize the heparin removal. The optimized protocol was pre-validated to determine the effectiveness of heparin plasma:ECT treatment to restore the PRNT titers as compared to serum samples. The validation and comparative performance was carried out by using a large range of serum vs heparin plasma:ECT 1:2 paired samples obtained from unvaccinated and 17DD-YFV primary vaccinated subjects. Altogether, the findings support the use of heparin plasma:ECT samples for accurate measurement of anti-YFV neutralizing antibodies. Copyright © 2017 Elsevier B.V. All rights reserved.

Pretreatment HIV Drug Resistance and HIV-1 Subtype C Are Independently Associated With Virologic Failure: Results From the Multinational PEARLS (ACTG A5175) Clinical Trial

PubMed Central

Kantor, Rami; Smeaton, Laura; Vardhanabhuti, Saran; Hudelson, Sarah E.; Wallis, Carol L.; Tripathy, Srikanth; Morgado, Mariza G.; Saravanan, Shanmugham; Balakrishnan, Pachamuthu; Reitsma, Marissa; Hart, Stephen; Mellors, John W.; Halvas, Elias; Grinsztejn, Beatriz; Hosseinipour, Mina C.; Kumwenda, Johnstone; La Rosa, Alberto; Lalloo, Umesh G.; Lama, Javier R.; Rassool, Mohammed; Santos, Breno R.; Supparatpinyo, Khuanchai; Hakim, James; Flanigan, Timothy; Kumarasamy, Nagalingeswaran; Campbell, Thomas B.; Eshleman, Susan H.

2015-01-01

Background. Evaluation of pretreatment HIV genotyping is needed globally to guide treatment programs. We examined the association of pretreatment (baseline) drug resistance and subtype with virologic failure in a multinational, randomized clinical trial that evaluated 3 antiretroviral treatment (ART) regimens and included resource-limited setting sites. Methods. Pol genotyping was performed in a nested case-cohort study including 270 randomly sampled participants (subcohort), and 218 additional participants failing ART (case group). Failure was defined as confirmed viral load (VL) >1000 copies/mL. Cox proportional hazards models estimated resistance–failure association. Results. In the representative subcohort (261/270 participants with genotypes; 44% women; median age, 35 years; median CD4 cell count, 151 cells/µL; median VL, 5.0 log10 copies/mL; 58% non-B subtypes), baseline resistance occurred in 4.2%, evenly distributed among treatment arms and subtypes. In the subcohort and case groups combined (466/488 participants with genotypes), used to examine the association between resistance and treatment failure, baseline resistance occurred in 7.1% (9.4% with failure, 4.3% without). Baseline resistance was significantly associated with shorter time to virologic failure (hazard ratio [HR], 2.03; P = .035), and after adjusting for sex, treatment arm, sex–treatment arm interaction, pretreatment CD4 cell count, baseline VL, and subtype, was still independently associated (HR, 2.1; P = .05). Compared with subtype B, subtype C infection was associated with higher failure risk (HR, 1.57; 95% confidence interval [CI], 1.04–2.35), whereas non-B/C subtype infection was associated with longer time to failure (HR, 0.47; 95% CI, .22–.98). Conclusions. In this global clinical trial, pretreatment resistance and HIV-1 subtype were independently associated with virologic failure. Pretreatment genotyping should be considered whenever feasible. Clinical Trials Registration. NCT00084136. PMID:25681380

Optimization of PMAxx pretreatment to distinguish between human norovirus with intact and altered capsids in shellfish and sewage samples.

PubMed

Randazzo, Walter; Khezri, Mohammad; Ollivier, Joanna; Le Guyader, Françoise S; Rodríguez-Díaz, Jesús; Aznar, Rosa; Sánchez, Gloria

2018-02-02

Shellfish contamination by human noroviruses (HuNoVs) is a serious health and economic problem. Recently an ISO procedure based on RT-qPCR for the quantitative detection of HuNoVs in shellfish has been issued, but these procedures cannot discriminate between inactivated and potentially infectious viruses. The aim of the present study was to optimize a pretreatment using PMAxx to better discriminate between intact and heat-treated HuNoVs in shellfish and sewage. To this end, the optimal conditions (30min incubation with 100μM of PMAxx and 0.5% of Triton, and double photoactivation) were applied to mussels, oysters and cockles artificially inoculated with thermally-inactivated (99°C for 5min) HuNoV GI and GII. This pretreatment reduced the signal of thermally-inactivated HuNoV GI in cockles and HuNoV GII in mussels by >3 log. Additionally, this pretreatment reduced the signal of thermally-inactivated HuNoV GI and GII between 1 and 1.5 log in oysters. Thermal inactivation of HuNoV GI and GII in PBS, sewage and bioaccumulated oysters was also evaluated by the PMAxx-Triton pretreatment. Results showed significant differences between reductions observed in the control and PMAxx-treated samples in PBS following treatment at 72 and 95°C for 15min. In sewage, the RT-qPCR signal of HuNoV GI was completely removed by the PMAxx pretreatment after heating at 72 and 95°C, while the RT-qPCR signal for HuNoV GII was completely eliminated only at 95°C. Finally, the PMAxx-Triton pretreatment was applied to naturally contaminated sewage and oysters, resulting in most of the HuNoV genomes quantified in sewage and oyster samples (12 out of 17) corresponding to undamaged capsids. Although this procedure may still overestimate infectivity, the PMAxx-Triton pretreatment represents a step forward to better interpret the quantification of intact HuNoVs in complex matrices, such as sewage and shellfish, and it could certainly be included in the procedures based on RT-qPCR. Copyright © 2017 Elsevier B.V. All rights reserved.

Pretreatment tables predicting pathologic stage of locally advanced prostate cancer.

PubMed

Joniau, Steven; Spahn, Martin; Briganti, Alberto; Gandaglia, Giorgio; Tombal, Bertrand; Tosco, Lorenzo; Marchioro, Giansilvio; Hsu, Chao-Yu; Walz, Jochen; Kneitz, Burkhard; Bader, Pia; Frohneberg, Detlef; Tizzani, Alessandro; Graefen, Markus; van Cangh, Paul; Karnes, R Jeffrey; Montorsi, Francesco; van Poppel, Hein; Gontero, Paolo

2015-02-01

Pretreatment tables for the prediction of pathologic stage have been published and validated for localized prostate cancer (PCa). No such tables are available for locally advanced (cT3a) PCa. To construct tables predicting pathologic outcome after radical prostatectomy (RP) for patients with cT3a PCa with the aim to help guide treatment decisions in clinical practice. This was a multicenter retrospective cohort study including 759 consecutive patients with cT3a PCa treated with RP between 1987 and 2010. Retropubic RP and pelvic lymphadenectomy. Patients were divided into pretreatment prostate-specific antigen (PSA) and biopsy Gleason score (GS) subgroups. These parameters were used to construct tables predicting pathologic outcome and the presence of positive lymph nodes (LNs) after RP for cT3a PCa using ordinal logistic regression. In the model predicting pathologic outcome, the main effects of biopsy GS and pretreatment PSA were significant. A higher GS and/or higher PSA level was associated with a more unfavorable pathologic outcome. The validation procedure, using a repeated split-sample method, showed good predictive ability. Regression analysis also showed an increasing probability of positive LNs with increasing PSA levels and/or higher GS. Limitations of the study are the retrospective design and the long study period. These novel tables predict pathologic stage after RP for patients with cT3a PCa based on pretreatment PSA level and biopsy GS. They can be used to guide decision making in men with locally advanced PCa. Our study might provide physicians with a useful tool to predict pathologic stage in locally advanced prostate cancer that might help select patients who may need multimodal treatment. Copyright © 2014 European Association of Urology. Published by Elsevier B.V. All rights reserved.

Current Pretreatment Technologies for the Development of Cellulosic Ethanol and Biorefineries.

PubMed

Silveira, Marcos Henrique Luciano; Morais, Ana Rita C; da Costa Lopes, Andre M; Olekszyszen, Drielly Nayara; Bogel-Łukasik, Rafał; Andreaus, Jürgen; Pereira Ramos, Luiz

2015-10-26

Lignocellulosic materials, such as forest, agriculture, and agroindustrial residues, are among the most important resources for biorefineries to provide fuels, chemicals, and materials in such a way to substitute for, at least in part, the role of petrochemistry in modern society. Most of these sustainable biorefinery products can be produced from plant polysaccharides (glucans, hemicelluloses, starch, and pectic materials) and lignin. In this scenario, cellulosic ethanol has been considered for decades as one of the most promising alternatives to mitigate fossil fuel dependence and carbon dioxide accumulation in the atmosphere. However, a pretreatment method is required to overcome the physical and chemical barriers that exist in the lignin-carbohydrate composite and to render most, if not all, of the plant cell wall components easily available for conversion into valuable products, including the fuel ethanol. Hence, pretreatment is a key step for an economically viable biorefinery. Successful pretreatment method must lead to partial or total separation of the lignocellulosic components, increasing the accessibility of holocellulose to enzymatic hydrolysis with the least inhibitory compounds being released for subsequent steps of enzymatic hydrolysis and fermentation. Each pretreatment technology has a different specificity against both carbohydrates and lignin and may or may not be efficient for different types of biomasses. Furthermore, it is also desirable to develop pretreatment methods with chemicals that are greener and effluent streams that have a lower impact on the environment. This paper provides an overview of the most important pretreatment methods available, including those that are based on the use of green solvents (supercritical fluids and ionic liquids). © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tackling bioactive glass excessive in vitro bioreactivity: Preconditioning approaches for cell culture tests.

PubMed

Ciraldo, Francesca E; Boccardi, Elena; Melli, Virginia; Westhauser, Fabian; Boccaccini, Aldo R

2018-05-21

Bioactive glasses (BGs) are being increasingly considered for biomedical applications in bone and soft tissue replacement approaches thanks to their ability to form strong bonding with tissues. However, due to their high reactivity once in contact with water-based solutions BGs rapidly exchange ions with the surrounding environment leading in most cases to an undesired increase of the pH under static in vitro conditions (due to alkaline ion "burst release"), making difficult or even impossible to perform cell culture studies. Several pre-conditioning treatments have been therefore proposed in laboratories worldwide to limit this problem. This paper presents an overview of the different strategies that have been put forward to pre-treat BG samples to tackle the pH raise issue in order to enable cell biology studies. The paper also discusses the relevant criteria that determine the selection of the optimal pre-treatment depending on the BG composition and morphology (e.g. particles, scaffolds). Bioactive glasses (BGs), since their discovery in 1971 by L.L Hench, have been widely used for bone replacement and repair, and, more recently, they are becoming highly attractive for bone and soft tissue engineering applications. BGs have in fact the ability to form a strong bond with both hard and soft tissues once in contact with biological fluid. The enhanced interaction of BGs with the biological environment is based on their significant surface bioreactivity. This surface effect of BGs is, on the other hand, problematic for cell biology studies by standard (static) cell culture methods: an excessive bioreactivity leads in most cases to a rapid and dramatic increase of the pH of the surrounding medium, which results in cell death and makes cell culture tests on BG samples impossible. The BG research community has been aware of this for many years and numerous pre-treatments have been proposed by different groups worldwide to limit this problem. For the first time, we have reviewed in this paper the variety of surface preconditioning treatments that have been put forward over the years, we provide a summary of such pre-treatments used in laboratory practice, discussing and offering criteria that can be used for the determination of the optimal pre-treatment depending on BG composition and morphology of the sample tested (bulk, particulate, scaffolds). The information and discussion provided in this review should support best research practice when testing bioactive glasses in cell culture. Copyright © 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Hydrothermal pretreatment of palm oil empty fruit bunch

NASA Astrophysics Data System (ADS)

Simanungkalit, Sabar Pangihutan; Mansur, Dieni; Nurhakim, Boby; Agustin, Astrid; Rinaldi, Nino; Muryanto, Fitriady, Muhammad Ariffudin

2017-01-01

Hydrothermal pretreatment methods in 2nd generation bioethanol production more profitable to be developed, since the conventional pretreatment, by using acids or alkalis, is associated with the serious economic and environmental constraints. The current studies investigate hydrothermal pretreatment of palm oil empty fruit bunch (EFB) in a batch tube reactor system with temperature and time range from 160 to 240 C and 15 to 30 min, respectively. The EFB were grinded and separated into 3 different particles sizes i.e. 10 mesh, 18 mesh and 40 mesh, prior to hydrothermal pretreatment. Solid yield and pH of the treated EFB slurries changed over treatment severities. The chemical composition of EFB was greatly affected by the hydrothermal pretreatment especially hemicellulose which decreased at higher severity factor as determined by HPLC. Both partial removal of hemicellulose and migration of lignin during hydrothermal pretreatment caused negatively affect for enzymatic hydrolysis. This studies provided important factors for maximizing hydrothermal pretreatment of EFB.

An evaluation of dilute acid and ammonia fiber explosion pretreatment for cellulosic ethanol production.

PubMed

Mathew, Anil Kuruvilla; Parameshwaran, Binod; Sukumaran, Rajeev Kumar; Pandey, Ashok

2016-01-01

The challenge associated with cellulosic ethanol production is maximizing sugar yield at low cost. Current research is being focused to develop a pretreatment method to overcome biomass recalcitrance in an efficient way. This review is focused on two major pretreatments: dilute acid (DA) and ammonia fiber explosion (AFEX) pretreatment of corn stover and how these pretreatment cause morphological and chemical changes to corn stover in order to overcome the biomass recalcitrance. This review highlights the key differences of these two pretreatments based on compositional analysis, cellulose and its crystallinity, morphological changes, structural changes to lignin, enzymatic reactivity and enzyme adsorption onto pretreated solids and finally cellulosic ethanol production from the hydrolysate of DA and AFEX treated corn stover. Each stage of the process, AFEX pretreated corn stover was superior to DA treated corn stover. Copyright © 2015 Elsevier Ltd. All rights reserved.

Lime pretreatment of lignocellulosic biomass

NASA Astrophysics Data System (ADS)

Chang, Shushien

Lignocellulose is a valuable alternative energy source. The susceptibility of lignocellulosic biomass to enzymatic hydrolysis is constrained due to its structural features, so pretreatment is essential to enhance enzymatic digestibility. Of the chemicals used as pretreatment agents, it has been reported that alkalis improve biomass digestibility significantly. In comparison with other alkalis such as NaOH and ammonia, lime (calcium hydroxide) has many advantages; it is very inexpensive, is safe, and can be recovered by carbonating wash water. The effects of lime pretreatment were explored on switchgrass and poplar wood, representing herbaceous and woody biomass, respectively. The effects of pretreatment conditions (time, temperature, lime loading, water loading, particle size, and oxygen pressure) have been systematically studies. Lime alone enhances the digestibility of switchgrass significantly; under the recommended conditions, the 3-d total sugar (glucose + xylose) yields of lime-treated switchgrass were 7 times that of untreated sample. When treating poplar wood, lime must be combined with oxygen to achieve high digestibility; oxidative lime pretreatment increased the 3-d total sugar yield of poplar wood to 12 times that of untreated sample. In a fundamental study, to determine why lime pretreatment is effective, the effects of three structural features on enzymatic digestibility were studied: lignin content, acetyl content, and crystallinity index (CrI). Poplar wood was treated with peracetic acid, potassium hydroxide, and ball milling to produce model lignocelluloses with a broad spectrum of lignin contents, acetyl contents, and CrI, respectively. Enzymatic hydrolysis was performed on the model lignocelluloses to determine the digestibility. Correlations between lignin/carbohydrate ratio, acetyl/carbohydrate ratio, CrI and digestibility were developed. The 95% prediction intervals show that the correlations predict the 1-h and 3-d total sugar conversions of a biomass sample within a precision of 5% and 20%, respectively. The digestibility of a variety of lime-treated biomass and ball-milled alpha-cellulose was compared to the correlations determined from the model compounds. The agreement between the measured and predicted values shows that the correlations are satisfactory and the three structural features---lignin content, acetyl content, and CrI---are the major factors that determine enzymatic digestibility.

Application of Fourier transform near-infrared spectroscopy combined with high-performance liquid chromatography in rapid and simultaneous determination of essential components in crude Radix Scrophulariae.

PubMed

Li, Xiaomeng; Fang, Dansi; Cong, Xiaodong; Cao, Gang; Cai, Hao; Cai, Baochang

2012-12-01

A method is described using rapid and sensitive Fourier transform near-infrared spectroscopy combined with high-performance liquid chromatography-diode array detection for the simultaneous identification and determination of four bioactive compounds in crude Radix Scrophulariae samples. Partial least squares regression is selected as the analysis type and multiplicative scatter correction, second derivative, and Savitzky-Golay filter were adopted for the spectral pretreatment. The correlation coefficients (R) of the calibration models were above 0.96 and the root mean square error of predictions were under 0.028. The developed models were applied to unknown samples with satisfactory results. The established method was validated and can be applied to the intrinsic quality control of crude Radix Scrophulariae.

Sensitive ionization of non-volatile analytes using protein solutions as spray liquid in desorption electrospray ionization mass spectrometry.

PubMed

Zhu, Zhiqiang; Han, Jing; Zhang, Yan; Zhou, Yafei; Xu, Ning; Zhang, Bo; Gu, Haiwei; Chen, Huanwen

2012-12-15

Desorption electrospray ionization (DESI) is the most popular ambient ionization technique for direct analysis of complex samples without sample pretreatment. However, for many applications, especially for trace analysis, it is of interest to improve the sensitivity of DESI-mass spectrometry (MS). In traditional DESI-MS, a mixture of methanol/water/acetic acid is usually used to generate the primary ions. In this article, dilute protein solutions were electrosprayed in the DESI method to create multiply charged primary ions for the desorption ionization of trace analytes on various surfaces (e.g., filter paper, glass, Al-foil) without any sample pretreatment. The analyte ions were then detected and structurally characterized using a LTQ XL mass spectrometer. Compared with the methanol/water/acetic acid (49:49:2, v/v/v) solution, protein solutions significantly increased the signal levels of non-volatile compounds such as benzoic acid, TNT, o-toluidine, peptide and insulin in either positive or negative ion detection mode. For all the analytes tested, the limits of detection (LODs) were reduced to about half of the original values which were obtained using traditional DESI. The results showed that the signal enhancement is highly correlated with the molecular weight of the proteins and the selected solid surfaces. The proposed DESI method is a universal strategy for rapid and sensitive detection of trace amounts of strongly bound and/or non-volatile analytes, including explosives, peptides, and proteins. The results indicate that the sensitivity of DESI can be further improved by selecting larger proteins and appropriate solid surfaces. Copyright © 2012 John Wiley & Sons, Ltd.

Rapid analysis of composition and reactivity in cellulosic biomass feedstocks with near-infrared spectroscopy.

PubMed

Payne, Courtney E; Wolfrum, Edward J

2015-01-01

Obtaining accurate chemical composition and reactivity (measures of carbohydrate release and yield) information for biomass feedstocks in a timely manner is necessary for the commercialization of biofuels. Our objective was to use near-infrared (NIR) spectroscopy and partial least squares (PLS) multivariate analysis to develop calibration models to predict the feedstock composition and the release and yield of soluble carbohydrates generated by a bench-scale dilute acid pretreatment and enzymatic hydrolysis assay. Major feedstocks included in the calibration models are corn stover, sorghum, switchgrass, perennial cool season grasses, rice straw, and miscanthus. We present individual model statistics to demonstrate model performance and validation samples to more accurately measure predictive quality of the models. The PLS-2 model for composition predicts glucan, xylan, lignin, and ash (wt%) with uncertainties similar to primary measurement methods. A PLS-2 model was developed to predict glucose and xylose release following pretreatment and enzymatic hydrolysis. An additional PLS-2 model was developed to predict glucan and xylan yield. PLS-1 models were developed to predict the sum of glucose/glucan and xylose/xylan for release and yield (grams per gram). The release and yield models have higher uncertainties than the primary methods used to develop the models. It is possible to build effective multispecies feedstock models for composition, as well as carbohydrate release and yield. The model for composition is useful for predicting glucan, xylan, lignin, and ash with good uncertainties. The release and yield models have higher uncertainties; however, these models are useful for rapidly screening sample populations to identify unusual samples.

Improvement in shelf life of minimally processed cilantro leaves through integration of kinetin pretreatment and packaging interventions: Studies on microbial population dynamics, biochemical characteristics and flavour retention.

PubMed

Ranjitha, K; Shivashankara, K S; Sudhakar Rao, D V; Oberoi, Harinder Singh; Roy, T K; Bharathamma, H

2017-04-15

Effect of integrating optimized combination of pretreatment with packaging on shelf life of minimally processed cilantro leaves (MPCL) was appraised through analysis of their sensory attributes, biochemical characteristics, microbial population and flavour profile during storage. Minimally pretreated cilantro leaves pretreated with 50ppm kinetin and packed in 25μ polypropylene bags showed a shelf life of 21days. Optimized combination helped in efficiently maintaining sensory parameters, flavour profile, and retention of antioxidants in MPCL until 21days. Studies conducted on the effect of optimized combination on microbial population and flavour profile revealed that among different microorganisms, pectinolysers had a significant effect on spoilage of MPCL and their population of ⩽3.59logcfu/g was found to be acceptable. Principal component analysis of headspace volatiles revealed that (E)-2-undecenal, (E)-2-hexadecenal, (E)-2-tetradecenal & (E)-2-tetradecen-1-ol in stored samples clustered with fresh samples and therefore, could be considered as freshness indicators for MPCL. Copyright © 2016 Elsevier Ltd. All rights reserved.

Study of thermal pre-treatment on anaerobic digestion of slaughterhouse waste by TGA-MS and FTIR spectroscopy.

PubMed

Rodríguez-Abalde, Ángela; Gómez, Xiomar; Blanco, Daniel; Cuetos, María José; Fernández, Belén; Flotats, Xavier

2013-12-01

Thermogravimetric analysis coupled to mass spectrometry (TGA-MS) and Fourier-transform infrared spectroscopy (FTIR) were used to describe the effect of pasteurization as a hygienic pre-treatment of animal by-products over biogas production. Piggery and poultry meat wastes were used as substrates for assessing the anaerobic digestion under batch conditions at mesophilic range. Poultry waste was characterized by high protein and carbohydrate content, while piggery waste presented a major fraction of fat and lower carbohydrate content. Results from anaerobic digestion tests showed a lower methane yield for the pre-treated poultry sample. TGA-MS and FTIR spectroscopy allowed the qualitative identification of recalcitrant nitrogen-containing compounds in the pre-treated poultry sample, produced by Maillard reactions. In the case of piggery waste, the recalcitrant compounds were not detected and its biodegradability test reported higher methane yield and production rates. TGA-MS and FTIR spectroscopy were demonstrated to be useful tools for explaining results obtained by anaerobic biodegradability test and in describing the presence of inhibitory problems.

Micro-pulverized extraction pretreatment for highly sensitive analysis of 11-nor-9-carboxy-Δ(9)-tetrahydrocannabinol in hair by liquid chromatography/tandem mass spectrometry.

PubMed

Kuwayama, Kenji; Miyaguchi, Hajime; Yamamuro, Tadashi; Tsujikawa, Kenji; Kanamori, Tatsuyuki; Iwata, Yuko T; Inoue, Hiroyuki

2015-11-30

A primary metabolite of Δ(9) -tetrahydrocannabinol, 11-nor-9-carboxytetrahydrocannabinol (THC-COOH), serves as an effective indicator for cannabis intake. According to the recommendations of the Society of Hair Testing, at least 0.2 pg/mg of THC-COOH (cut-off level) must be present in a hair sample to constitute a positive result in a drug test. Typically, hair is digested with an alkaline solution and is subjected to gas chromatography/tandem mass spectrometry (GC/MS/MS) with negative ion chemical ionization (NICI). It is difficult to quantify THC-COOH at the cut-off level using liquid chromatography/tandem mass spectrometry (LC/MS/MS) without acquisition of second-generation product ions in triple quadrupole-ion trap mass spectrometers, because large amounts of matrix components in the low-mass range produced by digestion interfere with the THC-COOH peak. Using the typical pretreatment method (alkaline dissolution) and micro-pulverized extraction (MPE) with a stainless bullet, we compared the quantification of THC-COOH using GC/MS/MS and LC/MS/MS. MPE reduced the amount of matrix components in the low-mass range and enabled the quantification of THC-COOH at 0.2 pg/mg using a conventional triple quadrupole liquid chromatograph coupled to a mass spectrometer. On the other hand, the MPE pretreatment was unsuitable for GC/MS/MS, probably due to matrix components in the high-mass range. The proper combination of pretreatments and instrumental analyses was shown to be important for detecting trace amounts of THC-COOH in hair. In MPE, samples can be prepared rapidly, and LC/MS/MS is readily available, unlike GC/MS/MS with NICI. The combination of MPE and LC/MS/MS might therefore be used in the initial screening for THC-COOH in hair prior to confirmatory analysis using GC/MS/MS with NICI. Copyright © 2015 John Wiley & Sons, Ltd.

Improved COD Measurements for Organic Content in Flowback Water with High Chloride Concentrations.

PubMed

Cardona, Isabel; Park, Ho Il; Lin, Lian-Shin

2016-03-01

An improved method was used to determine chemical oxygen demand (COD) as a measure of organic content in water samples containing high chloride content. A contour plot of COD percent error in the Cl(-)-Cl(-):COD domain showed that COD errors increased with Cl(-):COD. Substantial errors (>10%) could occur in low Cl(-):COD regions (<300) for samples with low (<10 g/L) and high chloride concentrations (>25 g/L). Applying the method to flowback water samples resulted in COD concentrations ranging in 130 to 1060 mg/L, which were substantially lower than the previously reported values for flowback water samples from Marcellus Shale (228 to 21 900 mg/L). It is likely that overestimations of COD in the previous studies occurred as result of chloride interferences. Pretreatment with mercuric sulfate, and use of a low-strength digestion solution, and the contour plot to correct COD measurements are feasible steps to significantly improve the accuracy of COD measurements.

[Study on the analytical methods of catechins in tea and green tea polyphenol samples by high performance liquid chromatography].

PubMed

Dai, J; Wang, H X; Chen, S W; Tang, J

2001-09-01

Hypersil BDS C18 and Zorbax SB C18, suitable to separate simultaneously seven kinds of catechins and caffeine, were screened out from seven brands of reversed-phase columns. Mobile phase was a solution of methanol-water-acetic acid (or trifluoro acetic acid). Seven kinds of catechins in tea samples from six places in China and three green tea polyphenol(GTP) samples from different producers were separated and determined in 30 min by isocratic and gradient elutions. The effects of mobile phase components and temperature of column on retention parameters of catechins and caffeine are reviewed. Chromatographic conditions and pretreatment methods of samples were optimized. Gallocatechin gallate(GCG) and (-)-catechin gallate(CG) were identified by electrospray ionization mass spectrometry(ESI-MS) and prepared by high performance liquid chromatography for quantitative analysis. The other catechins, (-)-epigallocatechin (EGC), (+)-catechin (D-C), (-)-epicatechin(EC), (-)-epigallocatechin gallate(EGCG), (-)-epicatechin gallate(ECG) were identified with standards.

Solvent-modified solid-phase microextraction for the determination of diazepam in human plasma samples by capillary gas chromatography.

PubMed

Krogh, M; Grefslie, H; Rasmussen, K E

1997-02-21

This paper describes microextraction and gas chromatographic analysis of diazepam from human plasma. The method was based on immobilisation of 1.5 microliters of 1-octanol on a polyacrylate-coated fiber designed for solid-phase microextraction. The solvent-modified fibre was used to extract diazepam from the samples. The plasma sample was pre-treated to release diazepam from the protein binding. The fibre was inserted into the modified plasma sample, adjusted to pH 5.5 an internal standard was added and the mixture was carefully stirred for 4 min. The fibre with the immobilised solvent and the enriched analytes was injected into the capillary gas chromatograph. The solvent and the extracted analytes were evaporated at 300 degrees C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicon capillary column and detected with a nitrogen-phosphorus detector. The method was shown to be reproducible with a detection limit of 0.10 nmol/ml in human plasma.

Nonhazardous Urine Pretreatment Method

NASA Technical Reports Server (NTRS)

Akse, James R.; Holtsnider, John T.

2012-01-01

A method combines solid phase acidification with two non-toxic biocides to prevent ammonia volatilization and microbial proliferation. The safe, non-oxidizing biocide combination consists of a quaternary amine and a food preservative. This combination has exhibited excellent stabilization of both acidified and unacidified urine. During pretreatment tests, composite urine collected from donors was challenged with a microorganism known to proliferate in urine, and then was processed using the nonhazardous urine pre-treatment method. The challenge microorganisms included Escherichia coli, a common gram-negative bacteria; Enterococcus faecalis, a ureolytic gram-positive bacteria; Candida albicans, a yeast commonly found in urine; and Aspergillus niger, a problematic mold that resists urine pre-treatment. Urine processed in this manner remained microbially stable for over 57 days. Such effective urine stabilization was achieved using non-toxic, non-oxidizing biocides at higher pH (3.6 to 5.8) than previous methods in use or projected for use aboard the International Space Station (ISS). ISS urine pretreatment methods employ strong oxidants including ozone and hexavalent chromium (Cr(VI)), a carcinogenic material, under very acidic conditions (pH = 1.8 to 2.4). The method described here offers a much more benign chemical environment than previous pretreatment methods, and will lower equivalent system mass (ESM) by reducing containment volume and mass, system complexity, and crew time needed to handle pre-treatment chemicals. The biocides, being non-oxidizing, minimize the potential for chemical reactions with urine constituents to produce volatile, airborne contaminants such as cyanogen chloride. Additionally, the biocides are active under significantly less acidic conditions than those used in the current system, thereby reducing the degree of required acidification. A simple flow-through solid phase acidification (SPA) bed is employed to overcome the natural buffering capacity of urine, and to lower the pH to levels that fix ammoniacal nitrogen in the non-volatile and highly water soluble NH4 + form. Citric acid, a highly soluble, solid tricarboxylic acid essential to cellular metabolism, and typically used as a food preservative, has also been shown to efficiently acidify urine in conjunction with non-oxidizing biocides to provide effective stabilization with respect to both microbial growth and ammonia volatilization.

The Effect of Acid Pre-Treatment using Acetic Acid and Nitric Acid in The Production of Biogas from Rice Husk during Solid State Anaerobic Digestion (SS-AD)

NASA Astrophysics Data System (ADS)

Nugraha, Winardi Dwi; Syafrudin; Keumala, Cut Fadhila; Matin, Hasfi Hawali Abdul; Budiyono

2018-02-01

Pretreatment during biogas production aims to assist in degradation of lignin contained in the rice husk. In this study, pretreatment which is used are acid and biological pretreatment. Acid pretreatment was performed using acetic acid and nitric acid with a variety levels of 3% and 5%. While biological pretreatment as a control variable. Acid pretreatment was conducted by soaking the rice straw for 24 hours with acid variation. The study was conducted using Solid State Anaerobic Digestion (SS-AD) with 21% TS. Biogas production was measured using water displacement method every two days for 60 days at room temperature conditions. The results showed that acid pretreatment gave an effect on the production of biogas yield. The yield of the biogas produced by pretreatment of acetic acid of 5% and 3% was 43.28 and 45.86 ml/gr.TS. While the results without pretreatment biogas yield was 29.51 ml/gr.TS. The results yield biogas produced by pretreatment using nitric acid of 5% and 3% was 12.14 ml/gr.TS and 21.85 ml/gr.TS. Results biogas yield with acetic acid pretreatment was better than the biogas yield results with nitric acid pretreatment.

Anaerobic digestion of organic fraction of municipal solid waste combining two pretreatment modalities, high temperature microwave and hydrogen peroxide.

PubMed

Shahriari, Haleh; Warith, Mostafa; Hamoda, Mohamed; Kennedy, Kevin J

2012-01-01

In order to enhance anaerobic digestion (AD) of the organic fraction of municipal solid waste (OFMSW), pretreatment combining two modalities, microwave (MW) heating in presence or absence of hydrogen peroxide (H(2)O(2)) were investigated. The main pretreatment variables affecting the characteristics of the OFMSW were temperature (T) via MW irradiation and supplemental water additions of 20% and 30% (SWA20 and SW30). Subsequently, the focus of this study was to evaluate mesophilic batch AD performance in terms of biogas production, as well as changes in the characteristics of the OFMSW post digestion. A high MW induced temperature range (115-175°C) was applied, using sealed vessels and a bench scale MW unit equipped with temperature and pressure controls. Biochemical methane potential (BMP) tests were conducted on the whole OFMSW as well as the liquid fractions. The whole OFMSW pretreated at 115°C and 145°C showed 4-7% improvement in biogas production over untreated OFMSW (control). When pretreated at 175°C, biogas production decreased due to formation of refractory compounds, inhibiting the digestion. For the liquid fraction of OFMSW, the effect of pretreatment on the cumulative biogas production (CBP) was more pronounced for SWA20 at 145°C, with a 26% increase in biogas production after 8days of digestion, compared to the control. When considering the increased substrate availability in the liquid fraction after MW pretreatment, a 78% improvement in biogas production vs. the control was achieved. Combining MW and H(2)O(2) modalities did not have a positive impact on OFMSW stabilization and enhanced biogas production. In general, all samples pretreated with H(2)O(2) displayed a long lag phase and the CBP was usually lower than MW irradiated only samples. First order rate constant was calculated. Copyright © 2011 Elsevier Ltd. All rights reserved.

Enhanced fermentable sugar production from kitchen waste using various pretreatments.

PubMed

Hafid, Halimatun Saadiah; Rahman, Nor'Aini Abdul; Md Shah, Umi Kalsom; Baharudin, Azhari Samsu

2015-06-01

The kitchen waste fraction in municipal solid waste contains high organic matter particularly carbohydrate that can contribute to fermentable sugar production for subsequent conversion to bioethanol. This study was carried out to evaluate the influence of single and combination pretreatments of kitchen waste by liquid hot water, mild acid pretreatment of hydrochloric acid (HCl) and sulphuric acid (H2SO4) and enzymatic hydrolysis (glucoamylase). The maximum total fermentable sugar produced after combination pretreatment by 1.5% HCl and glucoamylase consisted of 93.25 g/L glucose, 0.542 g/L sucrose, 0.348 g/L maltose, and 0.321 g/L fructose. The glucose released by the combination pretreatment method was 0.79 g glucose/g KW equivalent to 79% of glucose conversion. The effects of the pre-treatment on kitchen waste indicated that the highest solubilization was 40% by the combination method of 1.5% HCl and glucoamylase. The best combination pre-treatment gave concentrations of lactic acid, acetic acid, and propionic acid of 11.74 g/L, 6.77 g/L, and 1.02 g/L, respectively. The decrease of aliphatic absorbance bands of polysaccharides at 2851 and 2923 cm(-1) and the increase on structures of carbonyl absorbance bands at 1600 cm(-1) reflects the progress of the kitchen waste hydrolysis to fermentable sugars. Overall, 1.5% HCl and glucoamylase treatment was the most profitable process as the minimum selling price of glucose was USD 0.101/g kitchen waste. Therefore, the combination pretreatment method was proposed to enhance the production of fermentable sugar, particularly glucose from kitchen waste as the feedstock for bioethanol production. Copyright © 2015 Elsevier Ltd. All rights reserved.

Green methods of lignocellulose pretreatment for biorefinery development.

PubMed

Capolupo, Laura; Faraco, Vincenza

2016-11-01

Lignocellulosic biomass is the most abundant, low-cost, bio-renewable resource that holds enormous importance as alternative source for production of biofuels and other biochemicals that can be utilized as building blocks for production of new materials. Enzymatic hydrolysis is an essential step involved in the bioconversion of lignocellulose to produce fermentable monosaccharides. However, to allow the enzymatic hydrolysis, a pretreatment step is needed in order to remove the lignin barrier and break down the crystalline structure of cellulose. The present manuscript is dedicated to reviewing the most commonly applied "green" pretreatment processes used in bioconversion of lignocellulosic biomasses within the "biorefinery" concept. In this frame, the effects of different pretreatment methods on lignocellulosic biomass are described along with an in-depth discussion on the benefits and drawbacks of each method, including generation of potentially inhibitory compounds for enzymatic hydrolysis, effect on cellulose digestibility, and generation of compounds toxic for the environment, and energy and economic demand.

Comparative Evaluation of Three Homogenization Methods for Isolating Middle East Respiratory Syndrome Coronavirus Nucleic Acids From Sputum Samples for Real-Time Reverse Transcription PCR

PubMed Central

Yong, Dongeun; Ki, Chang-Seok; Kim, Jae-Seok; Seong, Moon-Woo; Lee, Hyukmin

2016-01-01

Background Real-time reverse transcription PCR (rRT-PCR) of sputum samples is commonly used to diagnose Middle East respiratory syndrome coronavirus (MERS-CoV) infection. Owing to the difficulty of extracting RNA from sputum containing mucus, sputum homogenization is desirable prior to nucleic acid isolation. We determined optimal homogenization methods for isolating viral nucleic acids from sputum. Methods We evaluated the following three sputum-homogenization methods: proteinase K and DNase I (PK-DNase) treatment, phosphate-buffered saline (PBS) treatment, and N-acetyl-L-cysteine and sodium citrate (NALC) treatment. Sputum samples were spiked with inactivated MERS-CoV culture isolates. RNA was extracted from pretreated, spiked samples using the easyMAG system (bioMérieux, France). Extracted RNAs were then subjected to rRT-PCR for MERS-CoV diagnosis (DiaPlex Q MERS-coronavirus, SolGent, Korea). Results While analyzing 15 spiked sputum samples prepared in technical duplicate, false-negative results were obtained with five (16.7%) and four samples (13.3%), respectively, by using the PBS and NALC methods. The range of threshold cycle (Ct) values observed when detecting upE in sputum samples was 31.1–35.4 with the PK-DNase method, 34.7–39.0 with the PBS method, and 33.9–38.6 with the NALC method. Compared with the control, which were prepared by adding a one-tenth volume of 1:1,000 diluted viral culture to PBS solution, the ranges of Ct values obtained by the PBS and NALC methods differed significantly from the mean control Ct of 33.2 (both P<0.0001). Conclusions The PK-DNase method is suitable for homogenizing sputum samples prior to RNA extraction. PMID:27374711

Biological pretreatment of corn stover with Phlebia brevispora NRRL-13108 for enhanced enzymatic hydrolysis and efficient ethanol production

USDA-ARS?s Scientific Manuscript database

Biological pretreatment of lignocellulosic biomass by white-rot fungus can represent a low-cost and eco-friendly alternative to harsh physical, chemical, or physico-chemical pretreatment methods to facilitate enzymatic hydrolysis. In this work, solid state cultivation of corn stover with Phlebia bre...

Restoration of severely weathered wood

Treesearch

R. Sam Williams; Mark Knaebe

2000-01-01

Severely weathered window units were used to test various restoration methods and pretreatments. Sanded and unsanded units were pretreated with a consolidant or water repellent preservative, finished with an oil- or latex-based paint system, and exposed outdoors near Madison, WI, for five years. Pretreatments were applied to both window sashes (stiles and rails) and...

Enhanced poly(L-malic acid) production from pretreated cane molasses by Aureobasidium pullulans in fed-batch fermentation.

PubMed

Xia, Jun; Xu, Jiaxing; Hu, Lei; Liu, Xiaoyan

2016-11-16

Poly(L-malic acid) (PMA) is a natural polyester with many attractive properties for biomedical application. However, the cost of PMA production is high when glucose is used as a carbon source. To solve this problem, cane molasses as a low-cost feedstock was applied for the production of PMA. Six pretreatment methods were applied to cane molasses before fermentation. Pretreatment with combined tricalcium phosphate, potassium ferrocyanide, and sulfuric acid (TPFSA) removed significant amounts of metal ions from cane molasses. The PMA concentration increased from 5.4 g/L (untreated molasses) to 36.9 g/L (TPFSA-pretreated molasses) after fermentation in shake flasks. A fed-batch fermentation strategy was then developed. In this method, TPFSA-pretreated cane molasses solution was continuously fed into the fermentor to maintain the total sugar concentration at 20 g/L. This technique generated approximately 95.4 g/L PMA with a productivity of 0.57 g/L/hr. The present study indicated that fed-batch fermentation using pretreated cane molasses is a feasible technique for producing high amounts of PMA.

Methods for producing and using densified biomass products containing pretreated biomass fibers

DOEpatents

Dale, Bruce E.; Ritchie, Bryan; Marshall, Derek

2015-05-26

A process is provided comprising subjecting a quantity of plant biomass fibers to a pretreatment to cause at least a portion of lignin contained within each fiber to move to an outer surface of said fiber, wherein a quantity of pretreated tacky plant biomass fibers is produced; and densifying the quantity of pretreated tacky plant biomass fibers to produce one or more densified biomass particulates, wherein said biomass fibers are densified without using added binder.

Fast and accurate preparation fatty acid methyl esters by microwave-assisted derivatization in the yeast Saccharomyces cerevisiae.

PubMed

Khoomrung, Sakda; Chumnanpuen, Pramote; Jansa-ard, Suwanee; Nookaew, Intawat; Nielsen, Jens

2012-06-01

We present a fast and accurate method for preparation of fatty acid methyl esters (FAMEs) using microwave-assisted derivatization of fatty acids present in yeast samples. The esterification of free/bound fatty acids to FAMEs was completed within 5 min, which is 24 times faster than with conventional heating methods. The developed method was validated in two ways: (1) through comparison with a conventional method (hot plate) and (2) through validation with the standard reference material (SRM) 3275-2 omega-3 and omega-6 fatty acids in fish oil (from the Nation Institute of Standards and Technology, USA). There were no significant differences (P>0.05) in yields of FAMEs with both validations. By performing a simple modification of closed-vessel microwave heating, it was possible to carry out the esterification in Pyrex glass tubes kept inside the closed vessel. Hereby, we are able to increase the number of sample preparations to several hundred samples per day as the time for preparation of reused vessels was eliminated. Pretreated cell disruption steps are not required, since the direct FAME preparation provides equally quantitative results. The new microwave-assisted derivatization method facilitates the preparation of FAMEs directly from yeast cells, but the method is likely to also be applicable for other biological samples.

Fully automated screening of veterinary drugs in milk by turbulent flow chromatography and tandem mass spectrometry

PubMed Central

Stolker, Alida A. M.; Peters, Ruud J. B.; Zuiderent, Richard; DiBussolo, Joseph M.

2010-01-01

There is an increasing interest in screening methods for quick and sensitive analysis of various classes of veterinary drugs with limited sample pre-treatment. Turbulent flow chromatography in combination with tandem mass spectrometry has been applied for the first time as an efficient screening method in routine analysis of milk samples. Eight veterinary drugs, belonging to seven different classes were selected for this study. After developing and optimising the method, parameters such as linearity, repeatability, matrix effects and carry-over were studied. The screening method was then tested in the routine analysis of 12 raw milk samples. Even without internal standards, the linearity of the method was found to be good in the concentration range of 50 to 500 µg/L. Regarding repeatability, RSDs below 12% were obtained for all analytes, with only a few exceptions. The limits of detection were between 0.1 and 5.2 µg/L, far below the maximum residue levels for milk set by the EU regulations. While matrix effects—ion suppression or enhancement—are obtained for all the analytes the method has proved to be useful for screening purposes because of its sensitivity, linearity and repeatability. Furthermore, when performing the routine analysis of the raw milk samples, no false positive or negative results were obtained. PMID:20379812

Effects of pretreatment on the surface chemistry and pore size properties of nitrogen functionalized and alkylated granular activated carbon

NASA Astrophysics Data System (ADS)

Chen, Jiajun; Zhai, Yunbo; Chen, Hongmei; Li, Caiting; Zeng, Guangming; Pang, Daoxiong; Lu, Pei

2012-12-01

In this paper, granular activated carbon (GAC) from coconut shell was pretreated by HNO3, H2O2 and urea-formaldehyde resin, respectively. Then the obtained materials were functionalized in the same way for nitrogen group, and then alkylated. Effects of pretreatment on the surface chemistry and pore size of modified GACs were studied. Surface area and micropore volume of modified GAC which pretreated by HNO3 were 723.88 m2/g and 0.229 cm3/g, respectively, while virgin GAC were 742.34 m2/g and 0.276 cm3/g. Surface area and micropore volume decrease of the modified GACs which pretreated by the others two methods were more drastically. The types of groups presented were analyzed by electrophoresis, Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Nsbnd CH3 group and Cdbnd N group were detected on the surfaces of these three kinds of modified GACs. Results of XPS showed that the nitrogen functions of modified GAC which pretreated by H2O2 was 4.07%, it was more than that of the others two pretreatment methods. However, the modified GAC which pretreated by urea-formaldehyde resin was fixed more pyridine structure, which structure percentage was 45.88%, in addition, there were more basic groups or charge on the surface than the others.

Enzymes and chelating agent in cotton pretreatment.

PubMed

Csiszár, E; Losonczi, A; Szakács, G; Rusznák, I; Bezúr, L; Reicher, J

2001-08-23

Desized cotton fabric and cotton seed-coat fragments (impurities) have been treated with commercial cellulase (Celluclast 1.5 L), hemicellulase-pectinase (Viscozyme 120 L) and xylanase (Pulpzyme HC) enzymes. Seed-coat fragments hydrolyzed much faster than the cotton fabric itself. This relative difference in hydrolysis rates makes possible a direct enzymatic removal of seed-coat fragments from desized cotton fabric. Addition of chelating agents such as ethylenediamine-tetra-acetic acid (EDTA) markedly enhanced the directed enzyme action. Pretreatments carried out in acidic solution at pH 5 increased the lightness of seed-coat fragments, contrary to the samples treated in neutral medium at pH 7. Alkaline scouring resulted in darker seed-coat fragments except for the samples pretreated with Pulpzyme HC plus EDTA. This effect is similar to that observed in the biobleaching process in pulp and paper industry.

Novel method for the determination of added annatto colour in extruded corn snack products.

PubMed

de Oliveira Rios, A; Mercadante, A Z

2004-02-01

There is considerable interest in determining the added levels of the natural dye annatto in foods like snack products, particularly because they are mostly consumed by young people. The objective was to use response surface methodology to develop a new method to analyse annatto in extruded snacks. A pretreatment of the samples was necessary, digesting the ground sample with alpha-amylase at room temperature. The pigment was extracted by shaking with ethyl acetate at room temperature, eight extractions being necessary for completion extract the pigment. Lipids were removed by alkaline saponification. Under these conditions, 100% of the bixin was converted into norbixin, which was then quantified by high-performance liquid chromatography. The method had a mean recovery of 97% and a coefficient of variation for duplicate analysis of 1%. Using this method, of the 13 commercial samples analysed, a parmesan cheese-flavoured snack product showed the highest level of dye expressed as norbixin (15.5 mg kg(-1)), whilst other brands of onion-flavoured snack products had the lowest levels (0.7 and 0.4 mg kg(-1), respectively).

Determination of the Degree of Substitution of Cationic Guar Gum by Headspace-Based Gas Chromatography during Its Synthesis.

PubMed

Wan, Xiaofang; Guo, Congbao; Feng, Jiarui; Yu, Teng; Chai, Xin-Sheng; Chen, Guangxue; Xie, Wei-Qi

2017-08-16

This study reports on a headspace-based gas chromatography (HS-GC) technique for determining the degree of substitution (DS) of cationic guar gum during the synthesis process. The method is based on the determination of 2,3-epoxypropyltrimethylammonium chloride in the process medium. After a modest pretreatment procedure, the sample was added to a headspace vial containing bicarbonate solution for measurement of evolved CO 2 by HS-GC. The results showed that the method had a good precision (relative standard deviation of <3.60%) and accuracy for the 2,3-epoxypropyltrimethylammonium chloride measurement, with recoveries in the range of 96-102%, matching with the data obtained by a reference method, and were within 12% of the values obtained by the more arduous Kjeldahl method for the calculated DS of cationic guar gum. The HS-GC method requires only a small volume of sample and, thus, is suitable for determining the DS of cationic guar gum in laboratory-scale process-related applications.

A novel pretreatment method combining sealing technique with direct injection technique applied for improving biosafety.

PubMed

Wang, Xinyu; Gao, Jing-Lin; Du, Chaohui; An, Jing; Li, MengJiao; Ma, Haiyan; Zhang, Lina; Jiang, Ye

2017-01-01

People today have a stronger interest in the risk of biosafety in clinical bioanalysis. A safe, simple, effective method of preparation is needed urgently. To improve biosafety of clinical analysis, we used antiviral drugs of adefovir and tenofovir as model drugs and developed a safe pretreatment method combining sealing technique with direct injection technique. The inter- and intraday precision (RSD %) of the method were <4%, and the extraction recoveries ranged from 99.4 to 100.7%. Meanwhile, the results showed that standard solution could be used to prepare calibration curve instead of spiking plasma, acquiring more accuracy result. Compared with traditional methods, the novel method not only improved biosecurity of the pretreatment method significantly, but also achieved several advantages including higher precision, favorable sensitivity and satisfactory recovery. With these highly practical and desirable characteristics, the novel method may become a feasible platform in bioanalysis.

Thermogravimetric analysis and kinetic modeling of low-transition-temperature mixtures pretreated oil palm empty fruit bunch for possible maximum yield of pyrolysis oil.

PubMed

Yiin, Chung Loong; Yusup, Suzana; Quitain, Armando T; Uemura, Yoshimitsu; Sasaki, Mitsuru; Kida, Tetsuya

2018-05-01

The impacts of low-transition-temperature mixtures (LTTMs) pretreatment on thermal decomposition and kinetics of empty fruit bunch (EFB) were investigated by thermogravimetric analysis. EFB was pretreated with the LTTMs under different duration of pretreatment which enabled various degrees of alteration to their structure. The TG-DTG curves showed that LTTMs pretreatment on EFB shifted the temperature and rate of decomposition to higher values. The EFB pretreated with sucrose and choline chloride-based LTTMs had attained the highest mass loss of volatile matter (78.69% and 75.71%) after 18 h of pretreatment. For monosodium glutamate-based LTTMs, the 24 h pretreated EFB had achieved the maximum mass loss (76.1%). Based on the Coats-Redfern integral method, the LTTMs pretreatment led to an increase in activation energy of the thermal decomposition of EFB from 80.00 to 82.82-94.80 kJ/mol. The activation energy was mainly affected by the demineralization and alteration in cellulose crystallinity after LTTMs pretreatment. Copyright © 2018 Elsevier Ltd. All rights reserved.

CdS nanoparticles-enhanced chemiluminescence and determination of baicalin in pharmaceutical preparations.

PubMed

Chen, Xiaolan; Tan, Xinmei; Wang, Jianxiu

2013-01-01

CdS nanoparticles (CdS NPs) of different sizes were synthesized by the citrate reduction method. It was found that CdS NPs could enhance the chemiluminescence (CL) of the luminol-potassium ferricyanide system and baicalin could inhibit CdS NPs-enhanced luminol-potassium ferricyanide CL signals in alkaline solution. Based on this inhibition, a flow-injection CL method was established for determination of baicalin in pharmaceutical preparations and human urine samples. Under optimized conditions, the linear range for determination of baicalin was 5.0 x 10(-6) to 1.0 x 10(-3) g/L. The detection limit at a signal-to-noise ratio of 3 was 1.7 x 10(-6) g/L. CL spectra, UV-visible spectra and transmission electron microscopy (TEM) were used to investigate the CL mechanism. The method described is simple, selective and obviates the need of extensive sample pretreatment. Copyright © 2012 John Wiley & Sons, Ltd.

Pretreatment technologies for industrial effluents: Critical review on bioenergy production and environmental concerns.

PubMed

Prabakar, Desika; Suvetha K, Subha; Manimudi, Varshini T; Mathimani, Thangavel; Kumar, Gopalakrishnan; Rene, Eldon R; Pugazhendhi, Arivalagan

2018-07-15

The implementation of different pretreatment techniques and technologies prior to effluent discharge is a direct result of the inefficiency of several existing wastewater treatment methods. A majority of the industrial sectors have known to cause severe negative effects on the environment. The five major polluting industries are the paper and pulp mills, coal manufacturing facilities, petrochemical, textile and the pharmaceutical sectors. Pretreatment methods have been widely used in order to lower the toxicity levels of effluents and comply with environmental standards. In this review, the possible environmental benefits and concerns of adopting different pretreatment technologies for renewable energy production and product/resource recovery has been reviewed and discussed. Copyright © 2018 Elsevier Ltd. All rights reserved.

Biodegradation of Enteromorpha prolifera by mangrove degrading micro-community with physical-chemical pretreatment.

PubMed

Zhao, Chao; Ruan, Lingwei

2011-11-01

The bacteria involved in the biodegradation of Enteromorpha prolifera (EP) are largely unknown, especially in offshore mangrove environments. In order to obtain the bacterial EP-degrading communities, sediments from a typical mangrove forest were sampled on the roots of mangrove in Dongzhai Port (Haikou, China). The sediments were enriched with crude EP powders as the sole carbon source. The bacterial composition of the resulting mangrove-degrading micro-community (MDMC), named D2-1, was analysed. With methods of plate cultivation and polymerase chain reaction-denaturing gradient gel electrophoresis and 16S rRNA library analysis, 18 bacteria belonging to nine genera were detected from this community. Among these detected bacteria, five major bands closely related to Bacillus, Marinobacter, Paenibacillus, Photobacterium, and Zhouia were determined. A novel two-step pretreatment for EP was proposed to lower the severity requirement of biodegraded pretreatment time. It consisted of a mild physical or chemical step (ultrasonic or H(2)O(2)) and a subsequent biological treatment with community D2-1. The combined treatment led to significant increases in the EP degradation. After combined treatment, the net yields of total soluble sugars and reducing sugars increased. The combined pretreatment of H(2)O(2) (2%, 48 h) and MDMC (7 days) was more effective than the treatment of MDMC only for 15 days. It could remarkably shorten the residence time and reduce the losses of carbohydrates. © Springer-Verlag 2011

Controlling microbial contamination during hydrolysis of AFEX-pretreated corn stover and switchgrass: Effects on hydrolysate composition, microbial response and fermentation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Serate, Jose; Xie, Dan; Pohlmann, Edward

Microbial conversion of lignocellulosic feedstocks into biofuels remains an attractive means to produce sustainable energy. It is essential to produce lignocellulosic hydrolysates in a consistent manner in order to study microbial performance in different feedstock hydrolysates. Because of the potential to introduce microbial contamination from the untreated biomass or at various points during the process, it can be difficult to control sterility during hydrolysate production. In this study, we compared hydrolysates produced from AFEX-pretreated corn stover and switchgrass using two different methods to control contamination: either by autoclaving the pretreated feedstocks prior to enzymatic hydrolysis, or by introducing antibiotics duringmore » the hydrolysis of non-autoclaved feedstocks. We then performed extensive chemical analysis, chemical genomics, and comparative fermentations to evaluate any differences between these two different methods used for producing corn stover and switchgrass hydrolysates. Autoclaving the pretreated feedstocks could eliminate the contamination for a variety of feedstocks, whereas the antibiotic gentamicin was unable to control contamination consistently during hydrolysis. Compared to the addition of gentamicin, autoclaving of biomass before hydrolysis had a minimal effect on mineral concentrations, and showed no significant effect on the two major sugars (glucose and xylose) found in these hydrolysates. However, autoclaving elevated the concentration of some furanic and phenolic compounds. Chemical genomics analyses using Saccharomyces cerevisiae strains indicated a high correlation between the AFEX-pretreated hydrolysates produced using these two methods within the same feedstock, indicating minimal differences between the autoclaving and antibiotic methods. Comparative fermentations with S. cerevisiae and Zymomonas mobilis also showed that autoclaving the AFEX-pretreated feedstocks had no significant effects on microbial performance in these hydrolysates. In conclusion, our results showed that autoclaving the pretreated feedstocks offered advantages over the addition of antibiotics for hydrolysate production. The autoclaving method produced a more consistent quality of hydrolysate.« less

Controlling microbial contamination during hydrolysis of AFEX-pretreated corn stover and switchgrass: Effects on hydrolysate composition, microbial response and fermentation

DOE PAGES

Serate, Jose; Xie, Dan; Pohlmann, Edward; ...

2015-11-14

Microbial conversion of lignocellulosic feedstocks into biofuels remains an attractive means to produce sustainable energy. It is essential to produce lignocellulosic hydrolysates in a consistent manner in order to study microbial performance in different feedstock hydrolysates. Because of the potential to introduce microbial contamination from the untreated biomass or at various points during the process, it can be difficult to control sterility during hydrolysate production. In this study, we compared hydrolysates produced from AFEX-pretreated corn stover and switchgrass using two different methods to control contamination: either by autoclaving the pretreated feedstocks prior to enzymatic hydrolysis, or by introducing antibiotics duringmore » the hydrolysis of non-autoclaved feedstocks. We then performed extensive chemical analysis, chemical genomics, and comparative fermentations to evaluate any differences between these two different methods used for producing corn stover and switchgrass hydrolysates. Autoclaving the pretreated feedstocks could eliminate the contamination for a variety of feedstocks, whereas the antibiotic gentamicin was unable to control contamination consistently during hydrolysis. Compared to the addition of gentamicin, autoclaving of biomass before hydrolysis had a minimal effect on mineral concentrations, and showed no significant effect on the two major sugars (glucose and xylose) found in these hydrolysates. However, autoclaving elevated the concentration of some furanic and phenolic compounds. Chemical genomics analyses using Saccharomyces cerevisiae strains indicated a high correlation between the AFEX-pretreated hydrolysates produced using these two methods within the same feedstock, indicating minimal differences between the autoclaving and antibiotic methods. Comparative fermentations with S. cerevisiae and Zymomonas mobilis also showed that autoclaving the AFEX-pretreated feedstocks had no significant effects on microbial performance in these hydrolysates. In conclusion, our results showed that autoclaving the pretreated feedstocks offered advantages over the addition of antibiotics for hydrolysate production. The autoclaving method produced a more consistent quality of hydrolysate.« less

Pretreatment of Eucalyptus in biphasic system for furfural production and accelerated enzymatic hydrolysis.

PubMed

Zhang, Xiudong; Bai, Yuanyuan; Cao, Xuefei; Sun, Runcang

2017-08-01

Herein, an efficient biphasic pretreatment process was developed to improve the production of furfural (FF) and glucose from Eucalyptus. The influence of formic acid and NaCl on FF production from xylose in water and various biphasic systems was investigated. Results showed that the addition of formic acid and NaCl significantly promoted the FF yield, and the biphasic system of MIBK (methyl isobutyl ketone)/water exhibited the best performance for FF production. Then the Eucalyptus was pretreated in the MIBK/water system, and a maximum FF yield of 82.0% was achieved at 180°C for 60min. Surface of the pretreated Eucalyptus became relatively rough and loose, and its crystallinity index increased obviously due to the removal of hemicelluloses and lignin. The pretreated Eucalyptus samples showed much higher enzymatic hydrolysis rates (26.2-70.7%) than the raw Eucalyptus (14.5%). Copyright © 2017 Elsevier Ltd. All rights reserved.

Exploring crystalline-structural variations of cellulose during alkaline pretreatment for enhanced enzymatic hydrolysis.

PubMed

Ling, Zhe; Chen, Sheng; Zhang, Xun; Xu, Feng

2017-01-01

The study aimed to explore the crystallinity and crystalline structure of alkaline pretreated cellulose. The enzymatic hydrolysis followed by pretreatment was conducted for measuring the efficiency of sugar conversion. For cellulose Iβ dominated samples, alkaline pretreatment (<8wt%) caused increased cellulose crystallinity and depolymerized hemicelluloses, that were superimposed to affect the enzymatic conversion to glucose. Varying crystallite sizes and lattice spacings indicated the separation of cellulose crystals during mercerization (8-12wt% NaOH). Completion of mercerization was proved under higher alkaline concentration (14-18wt% NaOH), leading to distortion of crystalline cellulose to some extent. Cellulose II crystallinity showed a stimulative impact on enzymatic hydrolysis due to the weakened hydrophobic interactions within cellulose chains. The current study may provide innovative explanations for enhanced enzymatic digestibility of alkaline pretreated lignocellulosic materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ozonolysis combined with ultrasound as a pretreatment of sugarcane bagasse: Effect on the enzymatic saccharification and the physical and chemical characteristics of the substrate.

PubMed

Perrone, Olavo Micali; Colombari, Felippe Mariano; Rossi, Jessika Souza; Moretti, Marcia Maria Souza; Bordignon, Sidnei Emilio; Nunes, Christiane da Costa Carreira; Gomes, Eleni; Boscolo, Mauricio; Da-Silva, Roberto

2016-10-01

Sugarcane bagasse (SCB) was treated in three stages using ozone oxidation (O), washing in an alkaline medium (B) and ultrasonic irradiation (U). The impact of each pretreatment stage on the physical structure of the SCB was evaluated by its chemical composition, using an infrared technique (FTIR-ATR), and using thermogravimetric analysis (TGA/DTG). The pretreatment sequence O, B, U provided a significant reduction of lignin and hemicellulose, which was confirmed by changes in the absorption bands corresponding to these compounds, when observed using infrared. Thermogravimetric analysis confirmed an increased thermal stability in the treated sample due to the removal of hemicellulose and extractives during the pretreatment. This pretreatment released 391mg glucose/g from treated SCB after the enzymatic hydrolysis, corresponding to a yield of 94% of the cellulose available. Copyright © 2016 Elsevier Ltd. All rights reserved.

SU-F-J-06: Optimized Patient Inclusion for NaF PET Response-Based Biopsies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roth, A; Harmon, S; Perk, T

Purpose: A method to guide mid-treatment biopsies using quantitative [F-18]NaF PET/CT response is being investigated in a clinical trial. This study aims to develop methodology to identify patients amenable to mid-treatment biopsy based on pre-treatment imaging characteristics. Methods: 35 metastatic prostate cancer patients had NaF PET/CT scans taken prior to the start of treatment and 9–12 weeks into treatment. For mid-treatment biopsy targeting, lesions must be at least 1.5 cm{sup 3} and located in a clinically feasible region (lumbar/sacral spine, pelvis, humerus, or femur). Three methods were developed based on number of lesions present prior to treatment: a feasibility-restricted method,more » a location-restricted method, and an unrestricted method. The feasibility restricted method only utilizes information from lesions meeting biopsy requirements in the pre-treatment scan. The unrestricted method accounts for all lesions present in the pre-treatment scan. For each method, optimized classification cutoffs for candidate patients were determined. Results: 13 of the 35 patients had enough lesions at the mid-treatment for biopsy candidacy. Of 1749 lesions identified in all 35 patients at mid-treatment, only 9.8% were amenable to biopsy. Optimizing the feasibility-restricted method required 4 lesions at pre-treatment meeting volume and region requirements for biopsy, resulting patient identification sensitivity of 0.8 and specificity of 0.7. Of 6 false positive patients, only one patient lacked lesions for biopsy. Restricting for location alone showed poor results (sensitivity 0.2 and specificity 0.3). The optimized unrestricted method required patients have at least 37 lesions in pretreatment scan, resulting in a sensitivity of 0.8 and specificity of 0.8. There were 5 false positives, only one lacked lesions for biopsy. Conclusion: Incorporating the overall pre-treatment number of NaF PET/CT identified lesions provided best prediction for identifying candidate patients for mid-treatment biopsy. This study provides validity for prediction-based inclusion criteria that can be extended to various clinical trial scenarios. Funded by Prostate Cancer Foundation.« less

Coupling corona discharge for ambient extractive ionization mass spectrometry.

PubMed

Hu, Bin; Zhang, Xinglei; Li, Ming; Peng, Xuejiao; Han, Jing; Yang, Shuiping; Ouyang, Yongzhong; Chen, Huanwen

2011-12-07

Unlike the extractive electrospray ionization (EESI) technique described elsewhere, a corona discharge instead of electrospray ionization has been utilized to charge a neutral solvent spray under ambient conditions for the generation of highly charged microdroplets, which impact a neutral sample plume for the extractive ionization of the analytes in raw samples without any sample pretreatment. Using the positive ion mode, molecular radical cations were easily generated for the detection of non-polar compounds (e.g., benzene, cyclohexane, etc.), while protonated molecular ions of polar compounds (e.g., acetonitrile, acetic ether) were readily produced for the detection. By dispensing the matrix in a relatively large space, this method tolerates highly complex matrices. For a given sample such as lily fragrances, more compounds were detected by the method established here than the EESI technique. An acceptable relative standard deviation (RSD 8.9%, n = 11) was obtained for the direct measurement of explosives (10 ppb) in waste water samples. The experimental data demonstrate that this method could simultaneously detect both polar and non-polar analytes with high sensitivity, showing promising applications for the rapid detection of a wide variety of compounds present in complex matrices.

Dialysis Extraction for Chromatography

NASA Technical Reports Server (NTRS)

Jahnsen, V. J.

1985-01-01

Chromatographic-sample pretreatment by dialysis detects traces of organic contaminants in water samples analyzed in field with minimal analysis equipment and minimal quantities of solvent. Technique also of value wherever aqueous sample and solvent must not make direct contact.

Physico-Chemical Properties and Biodegradability of Genetically Modified Populus trichocarpa and Pinus taeda

NASA Astrophysics Data System (ADS)

Edmunds, Charles Warren

Increasing concerns over greenhouse gas emissions and the finite supply of fossil fuels lead to the goal of utilizing lignocellulosic feedstocks for biofuels, platform chemicals, and biocomposites. Lignin is responsible for the recalcitrance of lignocellulosic biomass and is a major barrier to its deconstruction. Great progress has been made in mapping and modifying the lignin biosynthetic pathway. However, the link between the genetic modification, resulting chemical and physical properties of the wood, and how these properties influence the thermomechanical and recalcitrance to biological and chemical degradation needs further investigation. In this dissertation, the study of modified Populus trichocarpa and Pinus taeda were utilized to accomplish this goal. Thermo-mechanical properties of genetically modified P. trichocarpa with altered lignin content and/or lignin structure were measured with a series of tools including; dynamic mechanical analysis, nuclear magnetic resonance, and wet chemistry techniques. Results demonstrated lignin content and lignin structure likely influence the glass transition temperature (Tg), and that decreased lignin content and the corresponding higher proportion of cell wall carbohydrates may contribute to increased molecular mobility in the wood polymer structure. The effect of lignin biosynthetic pathway modification on biological degradation of these transgenic wood specimens was of interest. However, experimental methods for fungal treatment on small young greenhouse-grown wood specimens are not well established. Therefore, a project was undertaken to develop a method for fungal inoculation and incubation for these unique specimens. Several parameters were tested, and a fungal treatment method was identified with sufficient weight loss after decay and significant reduction in variation of weight loss between replicates compared to previous experiments by direct inoculation of wood with liquid malt extract fungal culture. Utilizing the fungal treatment method which was developed, fungal pretreatment as a potential low-input and environmentally-friendly alternative to conventional pretreatment methods was tested using the white-rot fungus, Ceriporiopsis subvermispora, on wildtype and transgenic P. trichocarpa. In addition to fungal treatment, hot water and dilute acid treatments followed by enzymatic hydrolysis was tested. Results showed no clear relationship between the initial lignin content or syringyl/guaiacyl lignin monomer ratio and weight loss due to fungal treatment. P-hydroxyphenyl lignin monomer degradation of up to 60% during the fungal treatment were observed in cinnamate 3-hydroxylase down-regulated genetic lines. It was demonstrated that fungal treatment in wildtype and several transgenic lines resulted in substantial improvements in sugar yields, up to 2.4-fold increase in glucose yield and 6.7-fold increase in xylose yield after enzymatic hydrolysis. However, some genetic lines showed little benefit from fungal pretreatment, and in general hot water and dilute acid pretreatments showed similar or increased glucose yield compared to fungal treatment. The goal of the last project was to characterize P. taeda which was genetically modified for S lignin production or decreased lignin content. In addition, the amenability to pretreatment and enzymatic hydrolysis were analyzed using hot water and dilute acid pretreatments followed by enzymatic hydrolysis. In the transgenic lines modified for production of syringyl lignin, Maule staining demonstrated the intermittent deposition of syringyl lignin in the secondary xylem, while thioacidolysis showed 13% concentration of S lignin, and solid state NMR demonstrated the occurrence of beta-O-4 linkages in S lignin units. In transgenic lines modified for reduced lignin content, lignin reduction up to 33% was observed, and pretreatment and enzymatic hydrolysis demonstrated increased cellulose conversion in lowlignin samples. These results highlight the potential of softwood to be a viable bioenergy/biochemical feedstock and opens up exciting new avenue of research.

Fungal pretreatment of willow sawdust and its combination with alkaline treatment for enhancing biogas production.

PubMed

Alexandropoulou, Maria; Antonopoulou, Georgia; Fragkou, Efsevia; Ntaikou, Ioanna; Lyberatos, Gerasimos

2017-12-01

In this study fungal pretreatment of willow sawdust (WSD) via the white rot fungi Leiotrametes menziesii and Abortiporus biennis was studied and the effect on fractionation of lignocellulosic biomass and biochemical methane potential (BMP), was evaluated. Scanning electron microscopy (SEM) and IR spectroscopy were used to investigate the changes in the structural characteristics of the pretreated WSD. Fungal pretreatment results revealed that A. biennis is more attractive, since it resulted in higher lignin degradation and lower holocellulose uptake. Samples of the 14th and 30th d of cultivation (i.e. the middle and the end of the pretreatment experiment) with both fungi were used for BMP tests and the effect of pretreatment duration was also evaluated. BMP increase by 31 and 43% was obtained due to the cultivation of WSD with A. biennis, for 14 and 30 d, respectively. In addition, combination of biological (after 30 d of cultivation) with alkaline (NaOH 20 g/100 gTS) pretreatment was performed, in order to assess the effect of the chemical agent on biologically pretreated WSD, in terms of lignocellulosic content and BMP. Combination of alkaline with fungal pretreatment led to high lignin degradation for both fungi, while the cellulose and hemicellulose removal efficiencies were higher for combined alkaline and L. menziesii pretreatment. The maximum BMP was observed for the combined alkaline and A. biennis pretreatment and was 12.5 and 50.1% higher than the respective alkaline and fungal pretreatment alone and 115% higher than the respective BMP of raw WSD. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparative Evaluation of Three Homogenization Methods for Isolating Middle East Respiratory Syndrome Coronavirus Nucleic Acids From Sputum Samples for Real-Time Reverse Transcription PCR.

PubMed

Sung, Heungsup; Yong, Dongeun; Ki, Chang Seok; Kim, Jae Seok; Seong, Moon Woo; Lee, Hyukmin; Kim, Mi Na

2016-09-01

Real-time reverse transcription PCR (rRT-PCR) of sputum samples is commonly used to diagnose Middle East respiratory syndrome coronavirus (MERS-CoV) infection. Owing to the difficulty of extracting RNA from sputum containing mucus, sputum homogenization is desirable prior to nucleic acid isolation. We determined optimal homogenization methods for isolating viral nucleic acids from sputum. We evaluated the following three sputum-homogenization methods: proteinase K and DNase I (PK-DNase) treatment, phosphate-buffered saline (PBS) treatment, and N-acetyl-L-cysteine and sodium citrate (NALC) treatment. Sputum samples were spiked with inactivated MERS-CoV culture isolates. RNA was extracted from pretreated, spiked samples using the easyMAG system (bioMérieux, France). Extracted RNAs were then subjected to rRT-PCR for MERS-CoV diagnosis (DiaPlex Q MERS-coronavirus, SolGent, Korea). While analyzing 15 spiked sputum samples prepared in technical duplicate, false-negative results were obtained with five (16.7%) and four samples (13.3%), respectively, by using the PBS and NALC methods. The range of threshold cycle (Ct) values observed when detecting upE in sputum samples was 31.1-35.4 with the PK-DNase method, 34.7-39.0 with the PBS method, and 33.9-38.6 with the NALC method. Compared with the control, which were prepared by adding a one-tenth volume of 1:1,000 diluted viral culture to PBS solution, the ranges of Ct values obtained by the PBS and NALC methods differed significantly from the mean control Ct of 33.2 (both P<0.0001). The PK-DNase method is suitable for homogenizing sputum samples prior to RNA extraction.

Application of pulsed electric field in the production of juice and extraction of bioactive compounds from blueberry fruits and their by-products.

PubMed

Bobinaitė, Ramunė; Pataro, Gianpiero; Lamanauskas, Nerijus; Šatkauskas, Saulius; Viškelis, Pranas; Ferrari, Giovanna

2015-09-01

The influence of Pulsed Electric Field (PEF) pre-treatment of blueberry fruits (Vaccinium myrtillus L.), both on the extraction yield and antioxidant properties of juice obtained by pressing and on the on the recovery of bioactive compounds from berry by-products (press cake) by extraction with solvent, was investigated. PEF treatments carried out at field strengths of 1, 3, and 5 kV/cm and an energy input of 10 kJ/kg achieved a cell disintegration index (Z p ) of 0.70, 0.80, and 0.87, respectively. Mechanical pressing (1.32 bar for 8 min) of PEF-treated berries (1, 3, and 5 kV/cm at 10 kJ/kg) significantly increased the juice yield (+28 %) compared with the untreated sample. The juice obtained from PEF pre-treated berries also had a significantly higher total phenolic content (+43 %), total anthocyanin content (+60 %) and antioxidant activity (+31 %). However, PEF treatment intensity higher than 1 kV/cm did not significantly improve the quantitative or qualitative characteristics of the juice. Compared to the untreated sample, higher amounts of total phenolics (+63 %), total athocyanins (+78 %) and antioxidant activity (+65 %) were detected in the press cake extracts. PEF treatment of higher intensity resulted in better extractability of bioactive compounds from blueberry press cake. The results obtained from this study demonstrate the potential of PEF as a mild pre-treatment method to improve the efficiency of the industrial processing of berry fruits.

Dielectric barrier discharge plasma pretreatment on hydrolysis of microcrystalline cellulose

NASA Astrophysics Data System (ADS)

Huang, Fangmin; Long, Zhouyang; Liu, Sa; Qin, Zhenglong

2017-04-01

Dielectric barrier discharge (DBD) plasma was used as a pretreatment method for downstream hydrolysis of microcrystalline cellulose (MCC). The degree of polymerization (DP) of MCC decreased after it was pretreated by DBD plasma under a carrier gas of air/argon. The effectiveness of depolymerization was found to be influenced by the crystallinity of MCC when under the pretreatment of DBD plasma. With the addition of tert-butyl alcohol in the treated MCC water suspension solution, depolymerization effectiveness of MCC was inhibited. When MCC was pretreated by DBD plasma for 30 min, the total reducing sugar concentration (TRSC) and liquefaction yield (LY) of pretreated-MCC (PMCC) increased by 82.98% and 34.18% respectively compared with those for raw MCC.

Long-Term Accelerated Corrosion and Adhesion Assessment of CARC Prepared Aluminum Alloy 5059-H131 Using Three Different Surface Preparation Methods

DTIC Science & Technology

2008-08-01

as part of a complete coating system, as was the case in this study. Trivalent chromium pretreatments such as Metalast TCP-HF must provide additional...pretreatment conditions. The pretreatment conditions were abrasive blasted; a nonchromate pretreatment, Alodine 5200; or a commercial trivalent chromate...vehicle in accordance with the MIL-DTL-46027J (1) for its combination of desirable traits such as lighter weight, ease of manufacturing via welds

Thermal Pretreatment of Wood for Co-gasification/co-firing of Biomass and Coal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Ping; Howard, Bret; Hedges, Sheila

2013-10-29

Utilization of biomass as a co-feed in coal and biomass co-firing and co-gasification requires size reduction of the biomass. Reducing biomass to below 0.2 mm without pretreatment is difficult and costly because biomass is fibrous and compressible. Torrefaction is a promising thermal pretreatment process and has the advantages of increasing energy density, improving grindability, producing fuels with more homogenous compositions and hydrophobic behavior. Temperature is the most important factor for the torrefaction process. Biomass grindability is related to cell wall structure, thickness and composition. Thermal treatment such as torrefaction can cause chemical changes that significantly affect the strength of biomass.more » The objectives of this study are to understand the mechanism by which torrefaction improves the grindability of biomass and discuss suitable temperatures for thermal pretreatment for co-gasification/co-firing of biomass and coal. Wild cherry wood was selected as the model for this study. Samples were prepared by sawing a single tangential section from the heartwood and cutting it into eleven pieces. The samples were consecutively heated at 220, 260, 300, 350, 450 and 550⁰C for 0.5 hr under flowing nitrogen in a tube furnace. Untreated and treated samples were characterized for physical properties (color, dimensions and weight), microstructural changes by SEM, and cell wall composition changes and thermal behaviors by TGA and DSC. The morphology of the wood remained intact through the treatment range but the cell walls were thinner. Thermal treatments were observed to decompose the cell wall components. Hemicellulose decomposed over the range of ~200 to 300⁰C and resulted in weakening of the cell walls and subsequently improved grindability. Furthermore, wood samples treated above 300⁰C lost more than 39% in mass. Therefore, thermal pretreatment above the hemicelluloses decomposition temperature but below 300⁰C is probably sufficient to improve grindability and retain energy value.« less

Application of dried blood spot cards to determine olive oil phenols (hydroxytyrosol metabolites) in human blood.

PubMed

de Las Hazas, María Carmen López; Motilva, Maria José; Piñol, Carme; Macià, Alba

2016-10-01

In this study, a fast and simple blood sampling and sample pre-treatment method based on the use of the dried blood spot (DBS) cards and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) for the quantification of olive oil phenolic metabolites in human blood was developed and validated. After validation, the method was applied to determine hydroxytyrosol metabolites in human blood samples after the acute intake of an olive oil phenolic extract. Using the FTA DMPK-A DBS card under optimum conditions, with 20µL as the blood solution volume, 100µL of methanol/Milli-Q water (50/50, v/v) as the extraction solvent and 7 disks punched out from the card, the main hydroxytyrosol metabolites (hydroxytyrosol-3-O-sulphate and hydroxytyrosol acetate sulphate) were identified and quantified. The developed methodology allowed detecting and quantifying the generated metabolites at low μM levels. The proposed method is a significant improvement over existing methods to determine phenolic metabolites circulating in blood and plasma samples, thus making blood sampling possible with the volunteer pricking their own finger, and the subsequent storage of the blood in the DBS cards prior to chromatographic analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

The thin-layer drying characteristics of sewage sludge by the appropriate foaming pretreatment.

PubMed

Wang, Hui-Ling; Yang, Zhao-Hui; Huang, Jing; Wang, Li-Ke; Gou, Cheng-Liu; Yan, Jing-Wu; Yang, Jian

2014-01-01

As dewatered sludge is highly viscous and sticky, the combination of foaming pretreatment and drying process seems to be an alternative method to improve the drying performance of dewatered sludge. In this study, CaO addition followed by mechanical whipping was employed for foaming the dewatered sludge. It was found that the foams were stable and the diameters of bubbles mainly ranged from 0.1 to 0.3 mm. The drying experiments were carried out in a drying oven in the convective mode. The results indicated that foamed sludge at 0.70 g/cm(3) had the best drying performance at each level of temperature, which could save 35-45% drying time to reach 20% moisture content compared with the non-foamed sludge. The drying rate of foamed sludge at 0.70 g/cm(3) was improved with the increasing of drying temperature. The impact of sample thickness on drying rate was not obvious when the sample thickness increased from 2 to 8 mm. Different mathematical models were used for the simulation of foamed sludge drying curves. The Wang and Singh model represented the drying characteristics better than other models with coefficient of determination values over 0.99.