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.

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.

A Novel Pretreatment-Free Duplex Chamber Digital PCR Detection System for the Absolute Quantitation of GMO Samples.

PubMed

Zhu, Pengyu; Wang, Chenguang; Huang, Kunlun; Luo, Yunbo; Xu, Wentao

2016-03-18

Digital polymerase chain reaction (PCR) has developed rapidly since it was first reported in the 1990s. However, pretreatments are often required during preparation for digital PCR, which can increase operation error. The single-plex amplification of both the target and reference genes may cause uncertainties due to the different reaction volumes and the matrix effect. In the current study, a quantitative detection system based on the pretreatment-free duplex chamber digital PCR was developed. The dynamic range, limit of quantitation (LOQ), sensitivity and specificity were evaluated taking the GA21 event as the experimental object. Moreover, to determine the factors that may influence the stability of the duplex system, we evaluated whether the pretreatments, the primary and secondary structures of the probes and the SNP effect influence the detection. The results showed that the LOQ was 0.5% and the sensitivity was 0.1%. We also found that genome digestion and single nucleotide polymorphism (SNP) sites affect the detection results, whereas the unspecific hybridization within different probes had little side effect. This indicated that the detection system was suited for both chamber-based and droplet-based digital PCR. In conclusion, we have provided a simple and flexible way of achieving absolute quantitation for genetically modified organism (GMO) genome samples using commercial digital PCR detection systems.

A Novel Pretreatment-Free Duplex Chamber Digital PCR Detection System for the Absolute Quantitation of GMO Samples

PubMed Central

Zhu, Pengyu; Wang, Chenguang; Huang, Kunlun; Luo, Yunbo; Xu, Wentao

2016-01-01

Digital polymerase chain reaction (PCR) has developed rapidly since it was first reported in the 1990s. However, pretreatments are often required during preparation for digital PCR, which can increase operation error. The single-plex amplification of both the target and reference genes may cause uncertainties due to the different reaction volumes and the matrix effect. In the current study, a quantitative detection system based on the pretreatment-free duplex chamber digital PCR was developed. The dynamic range, limit of quantitation (LOQ), sensitivity and specificity were evaluated taking the GA21 event as the experimental object. Moreover, to determine the factors that may influence the stability of the duplex system, we evaluated whether the pretreatments, the primary and secondary structures of the probes and the SNP effect influence the detection. The results showed that the LOQ was 0.5% and the sensitivity was 0.1%. We also found that genome digestion and single nucleotide polymorphism (SNP) sites affect the detection results, whereas the unspecific hybridization within different probes had little side effect. This indicated that the detection system was suited for both chamber-based and droplet-based digital PCR. In conclusion, we have provided a simple and flexible way of achieving absolute quantitation for genetically modified organism (GMO) genome samples using commercial digital PCR detection systems. PMID:26999129

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.

Facile preparation of nitrogen-doped porous carbon from waste tobacco by a simple pre-treatment process and their application in electrochemical capacitor and CO{sub 2} capture

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

Sha, Yunfei; Lou, Jiaying; Bai, Shizhe

2015-04-15

Highlights: • A pre-treatment process is used to prepared N-doped carbon from waste biomass. • Waste tobaccos, which are limited for the disposal, are used as the raw materials. • The product shows a specific surface area and nitrogen content. • Its electrochemical performance is better than commercial activated carbon. • Its CO{sub 2} sorption performance is also better than commercial activated carbon. - Abstract: Preparing nitrogen-doped porous carbons directly from waste biomass has received considerable interest for the purpose of realizing the atomic economy. In this study, N-doped porous carbons have been successfully prepared from waste tobaccos (WT) bymore » a simple pre-treatment process. The sample calcinated at 700 °C (WT-700) shows a micro/meso-porous structures with a BET surface area of 1104 m{sup 2} g{sup −1} and a nitrogen content of ca. 19.08 wt.% (EDS). Performance studies demonstrate that WT-700 displays 170 F g{sup −1} electrocapacitivity at a current density of 0.5 A g{sup −1} (in 6 M KOH), and a CO{sub 2} capacity of 3.6 mmol g{sup −1} at 0 °C and 1 bar, and a selectivity of ca. 32 for CO{sub 2} over N{sub 2} at 25 °C. Our studies indicate that it is feasible to prepare N-enriched porous carbons from waste natural crops by a pre-treatment process for potential industrial application.« less

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.

Micro-Spectroscopic Imaging of Lignin-Carbohydrate Complexes in Plant Cell Walls and Their Migration During Biomass Pretreatment

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

Zeng, Yining; Zhao, Shuai; Wei, Hui

2015-04-27

In lignocellulosic biomass, lignin is the second most abundant biopolymer. In plant cell walls, lignin is associated with polysaccharides to form lignin-carbohydrate complexes (LCC). LCC have been considered to be a major factor that negatively affects the process of deconstructing biomass to simple sugars by cellulosic enzymes. Here, we report a micro-spectroscopic approach that combines fluorescence lifetime imaging microscopy and Stimulated Raman Scattering microscopy to probe in situ lignin concentration and conformation at each cell wall layer. This technique does not require extensive sample preparation or any external labels. Using poplar as a feedstock, for example, we observe variation ofmore » LCC in untreated tracheid poplar cell walls. The redistribution of LCC at tracheid poplar cell wall layers is also investigated when the chemical linkages between lignin and hemicellulose are cleaved during pretreatment. Our study would provide new insights into further improvement of the biomass pretreatment process.« 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.

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.

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.

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.

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.

A simple, rapid and novel method based on salting-out assisted liquid-liquid extraction for ochratoxin A determination in beer samples prior to ultra-high performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Mariño-Repizo, Leonardo; Goicoechea, Hector; Raba, Julio; Cerutti, Soledad

2018-06-07

A novel, simple, easy and cheap sample treatment strategy based on salting-out assisted liquid-liquid extraction (SALLE) for ochratoxin A (OTA) ultra-trace analysis in beer samples using ultra-high performance liquid chromatography-tandem mass spectrometry determination was developed. The factors involved in the efficiency of pretreatment were studied employing factorial design in the screening phase and the optimal conditions of the significant variables on the analytical response were evaluated using a central composite face-centred design (CCF). Consequently, the amount of salt ((NH 4 ) 2 SO 4 ), together with the volumes of sample, hydrophilic (acetone) and nonpolar (toluene) solvents, and times of vortexing and centrifugation were optimized. Under optimized conditions, the limits of detection (LOD) and quantification (LOQ) were 0.02 µg l -1 and 0.08 µg l -1 respectively. OTA extraction recovery by SALLE was approximately 90% (0.2 µg l -1 ). Furthermore, the methodology was in agreement with EU Directive requirements and was successfully applied for analysis of beer samples.

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.

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.

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.

Bienzymatic Biosensor for Rapid Detection of Aspartame by Flow Injection Analysis

PubMed Central

Radulescu, Maria-Cristina; Bucur, Bogdan; Bucur, Madalina-Petruta; Radu, Gabriel Lucian

2014-01-01

A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX), carboxyl esterase (CaE) and bovine serum albumin (BSA) were immobilised with glutaraldehyde (GA) onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC). The biosensor response was fast. The sample throughput using a flow injection analysis (FIA) system was 40 h−1 with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 μM for methanol and 0.2 μM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples) without any pre-treatment step prior to measurement. PMID:24412899

Bienzymatic biosensor for rapid detection of aspartame by flow injection analysis.

PubMed

Radulescu, Maria-Cristina; Bucur, Bogdan; Bucur, Madalina-Petruta; Radu, Gabriel Lucian

2014-01-09

A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX), carboxyl esterase (CaE) and bovine serum albumin (BSA) were immobilised with glutaraldehyde (GA) onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC). The biosensor response was fast. The sample throughput using a flow injection analysis (FIA) system was 40 h⁻¹ with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 µM for methanol and 0.2 µM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples) without any pre-treatment step prior to measurement.

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.

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.

Extractive electrospray ionization mass spectrometry toward in situ analysis without sample pretreatment.

PubMed

Li, Ming; Hu, Bin; Li, Jianqiang; Chen, Rong; Zhang, Xie; Chen, Huanwen

2009-09-15

A homemade novel nanoextractive electrospray ionization (nanoEESI) source has been characterized for in situ mass spectrometric analysis of ambient samples without sample pretreatment. The primary ions generated using a nanospray emitter interact with the neutral sample plume created by manually nebulizing liquid samples, allowing production of the analyte ions in the spatial cross section of the nanoEESI source. The performance of nanoEESI is experimentally investigated by coupling the nanoEESI source to a commercial LTQ mass spectrometer for rapid analysis of various ambient samples using positive/negative ion detection modes. Compounds of interest in actual samples such as aerosol drug preparations, beverages, milk suspensions, farmland water, and groundwater were unambiguously detected using tandem nanoEESI ion trap mass spectrometry. The limit of detection was low picogram per milliliter levels for the compounds tested. Acceptable relative standard deviation (RSD) values (5-10%) were obtained for direct measurement of analytes in complex matrixes, providing linear dynamic signal responses using manual sample introduction. A single sample analysis was completed within 1.2 s. Requiring no sheath gas for either primary ion production or neutral sample introduction, the nanoEESI has advantages including readiness for miniaturization and integration, simple maintenance, easy operation, and low cost. The experimental data demonstrate that the nanoEESI is a promising tool for high-throughput, sensitive, quantitative, in situ analysis of ambient complex samples, showing potential applications for in situ analysis in multiple disciplines including but not limited to pharmaceutical analysis, food quality control, pesticides residue detection, and homeland security.

Sensitive and simple determination of zwitterionic morphine in human urine based on liquid-liquid micro-extraction coupled with surface-enhanced Raman spectroscopy.

PubMed

Yu, Borong; Cao, Chentai; Li, Pan; Mao, Mei; Xie, Qiwen; Yang, Liangbao

2018-08-15

Morphine, a kind of illicit drugs, is also one of the main heroin metabolites. In consideration of a noninvasive way to monitor and identify drug abuse during forensic cases, the urine samples are usually detected. Here, colloidal gold nanorods (Au NRs) were introduced to act as active substrate, because of the strong optical extinction and spectral tunability of the longitudinal surface plasmon resonance (SPR). Thus, well surface-enhanced Raman spectra of morphine even at low concentrations could be obtained by portable Raman spectrometer. For the complex matrix environment of urine, liquid-liquid micro-extraction (LLME), a simple and inexpensive pretreatment, was employed to avoid the interferences. And then, the coupled surface-enhanced Raman spectroscopy (SERS) can give full play to the advantages of high sensitivity and unique spectroscopic fingerprint. According to the zwitterionic structure and physicochemical parameters of morphine molecules, the pH value of urine sample was adjusted to about 9 by buffer solution (KOH/NaB 4 O 7 ) and the mixture of chloroform and isopropyl alcohol (V/V=9:1) was chosen as extractant. Moreover, such pretreatment was proved to be appropriate for separation and concentration of morphine from urine. The developed LLME-SERS method could provide a detection limit less than 1 ppm in the human urine environment and the whole process of detection just needed take 5-6 min. What's more, the results of urine samples from heroin users exhibited application value of the proposed technique. The excellent performance makes it promising to become a rapid, reliable, and on-spot analyzer, especially for public safety and healthcare. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

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.

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.

Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

PubMed Central

Kasiotis, Konstantinos M.; Souki, Helen; Tsakirakis, Angelos N.; Carageorgiou, Haris; Theotokatos, Spiridon A.; Haroutounian, Serkos A.; Machera, Kyriaki

2008-01-01

A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL) without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites fenoxon and fenthion–sulfoxide were also identified. PMID:19325792

UV-Surface Treatment of Fungal Resistant Polyether Polyurethane Film-Induced Growth of Entomopathogenic Fungi.

PubMed

Lando, Gabriela Albara; Marconatto, Letícia; Kessler, Felipe; Lopes, William; Schrank, Augusto; Vainstein, Marilene Henning; Weibel, Daniel Eduardo

2017-07-18

Synthetic polymers are the cause of some major environmental impacts due to their low degradation rates. Polyurethanes (PU) are widely used synthetic polymers, and their growing use in industry has produced an increase in plastic waste. A commercial polyether-based thermoplastic PU with hydrolytic stability and fungus resistance was only attacked by an entomopathogenic fungus, Metarhiziumanisopliae , when the films were pre-treated with Ultraviolet (UV) irradiation in the presence of reactive atmospheres. Water contact angle, Fourier transform infrared spectroscopy in attenuated total reflection mode (FTIR-ATR), scanning electron microscopy (SEM), and profilometer measurements were mainly used for analysis. Permanent hydrophilic PU films were produced by the UV-assisted treatments. Pristine polyether PU films incubated for 10, 30, and 60 days did not show any indication of fungal growth. On the contrary, when using oxygen in the UV pre-treatment a layer of fungi spores covered the sample, indicating a great adherence of the microorganisms to the polymer. However, if acrylic acid vapors were used during the UV pre-treatment, a visible attack by the entomopathogenic fungi was observed. SEM and FTIR-ATR data showed clear evidence of fungal development: growth and ramifications of hyphae on the polymer surface with the increase in UV pre-treatment time and fungus incubation time. The results indicated that the simple UV surface activation process has proven to be a promising alternative for polyether PU waste management.

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.

Study on methenamine detection in starch products through SERS technology

NASA Astrophysics Data System (ADS)

Cui, Yu; Qu, Zhou

2016-01-01

Using silver sol as a strengthened base, this paper concludes that l0ppb-0.1ppb methenamine aqueous solution has a better signal in 1052cm-1 Raman feature. And the lower limit of the aqueous solution is about 0.1ppb. Adding corresponding amount methenamine in vermicelli sample, the lower limit is about 10ppm. This is a safest and pollution-free detection process. Furthermore, the pretreatment process is simple, which will be finished in 20 minutes. Hence, it is better than other detection methods. SERS technology provides a simple, rapid and efficient detection method for field measurement and real time detection modulating disk of component, laser zooming system. Through the use of laser diode, Laser-beam riding guided system is likely to have smaller shape and very light.

Polymeric ionic liquid-based portable tip microextraction device for on-site sample preparation of water samples.

PubMed

Chen, Lei; Pei, Junxian; Huang, Xiaojia; Lu, Min

2018-06-05

On-site sample preparation is highly desired because it avoids the transportation of large-volume samples and ensures the accuracy of the analytical results. In this work, a portable prototype of tip microextraction device (TMD) was designed and developed for on-site sample pretreatment. The assembly procedure of TMD is quite simple. Firstly, polymeric ionic liquid (PIL)-based adsorbent was in-situ prepared in a pipette tip. After that, the tip was connected with a syringe which was driven by a bidirectional motor. The flow rates in adsorption and desorption steps were controlled accurately by the motor. To evaluate the practicability of the developed device, the TMD was used to on-site sample preparation of waters and combined with high-performance liquid chromatography with diode array detection to measure trace estrogens in water samples. Under the most favorable conditions, the limits of detection (LODs, S/N = 3) for the target analytes were in the range of 4.9-22 ng/L, with good coefficients of determination. Confirmatory study well evidences that the extraction performance of TMD is comparable to that of the traditional laboratory solid-phase extraction process, but the proposed TMD is more simple and convenient. At the same time, the TMD avoids complicated sampling and transferring steps of large-volume water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Comparison of some new pretreatment methods for second generation bioethanol production from wheat straw and water hyacinth.

PubMed

Guragain, Yadhu Nath; De Coninck, Joelle; Husson, Florence; Durand, Alain; Rakshit, Sudip Kumar

2011-03-01

Pretreatment of lignocellulosic residues like water hyacinth (WH) and wheat straw (WS) using crude glycerol (CG) and ionic liquids (IL) pretreatment was evaluated and compared with conventional dilute acid pretreatment (DAT) in terms of enzymatic hydrolysis yield and fermentation yield of pretreated samples. In the case of WS, 1-butyl-3-methylimidazolium acetate pretreatment was found to be the best method. The hydrolysis yields of glucose and total reducing sugars were 2.1 and 3.3 times respectively higher by IL pretreatment than DAT, while it was 1.4 and 1.9 times respectively higher with CG pretreatment. For WH sample, CG pretreatment was as effective as DAT and more effective than IL pretreatment regarding hydrolysis yield. The fermentation inhibition was not noticeable with both types of pretreatment methods and feedstocks. Besides, CG pretreatment was found as effective as pure glycerol pretreatment for both feedstocks. This opens up an attractive economic route for the utilization of CG. Copyright © 2010 Elsevier Ltd. All rights reserved.

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).

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 %.

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.

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.

Isolation of a significant fraction of non-phototroph diversity from a desert Biological Soil Crust

DOE PAGES

Nunes da Rocha, Ulisses; Cadillo-Quiroz, Hinsby; Karaoz, Ulas; ...

2015-04-14

Biological Soil Crusts (BSCs) are organosedimentary assemblages comprised of microbes and minerals in topsoil of terrestrial environments. BSCs strongly impact soil quality in dryland ecosystems (e.g., soil structure and nutrient yields) due to pioneer species such as Microcoleus vaginatus; phototrophs that produce filaments that bind the soil together, and support an array of heterotrophic microorganisms. These microorganisms in turn contribute to soil stability and biogeochemistry of BSCs. Non-cyanobacterial populations of BSCs are less well known than cyanobacterial populations. Therefore, we attempted to isolate a broad range of numerically significant and phylogenetically representative BSC aerobic heterotrophs. Combining simple pre-treatments (hydration ofmore » BSCs under dark and light) and isolation strategies (media with varying nutrient availability and protection from oxidative stress) we recovered 402 bacterial and one fungal isolate in axenic culture, which comprised 116 phylotypes (at 97% 16S rRNA gene sequence homology), 115 bacterial and one fungal. Each medium enriched a mostly distinct subset of phylotypes, and cultivated phylotypes varied due to the BSC pre-treatment. The fraction of the total phylotype diversity isolated, weighted by relative abundance in the community, was determined by the overlap between isolate sequences and OTUs reconstructed from metagenome or metatranscriptome reads. Together, more than 8% of relative abundance of OTUs in the metagenome was represented by our isolates, a cultivation efficiency much larger than typically expected from most soils. We conclude that simple cultivation procedures combined with specific pre-treatment of samples afford a significant reduction in the culturability gap, enabling physiological and metabolic assays that rely on ecologically relevant axenic cultures.« less

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.

A rapid and ultrasensitive SERRS assay for histidine and tyrosine based on azo coupling.

PubMed

Sui, Huimin; Wang, Yue; Yu, Zhi; Cong, Qian; Han, Xiao Xia; Zhao, Bing

2016-10-01

A simple and highly sensitive surface-enhanced resonance Raman scattering (SERRS)-based approach coupled with azo coupling reaction has been put forward for quantitative analysis of histidine and tyrosine. The SERRS-based assay is simple and rapid by mixing the azo reaction products with silver nanoparticles (AgNPs) for measurements within 2min. The limits of detection (LODs) of the method are as low as 4.33×10(-11) and 8.80×10(-11)M for histidine and tyrosine, respectively. Moreover, the SERRS fingerprint information specific to corresponding amino acids guarantees the selective detection for the target histidine and tyrosine. The results from serum indicated the potential application of the proposed approach into biological samples. Compared with the methods ever reported, the main advantages of this methodology are simpleness, rapidity without time-consuming separation or pretreatment steps, high sensitivity, selectivity and the potential for determination of other molecules containing imidazole or phenol groups. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Rapid detection of acetamiprid in foods using surface-enhanced Raman spectroscopy (SERS).

PubMed

Wijaya, Wisiani; Pang, Shintaro; Labuza, Theodore P; He, Lili

2014-04-01

Acetamiprid is a neonicotinoid pesticide that is commonly used in modern farming. Acetamiprid residue in food commodities can be a potential harm to human and has been implicated in the honey bee hive die off crisis. In this study, we developed rapid, simple, and sensitive methods to detect acetamiprid in apple juice and on apple surfaces using surface-enhanced Raman spectroscopy (SERS). No pretreatment of apple juice sample was performed. A simple surface swab method was used to recover acetamiprid from the apple surface. Samples were incubated with silver dendrites for several minutes and SERS spectra were taken directly from the silver surface. Detection of a set of 5 apple juice samples can be done within 10 min. The swab-SERS method took 15 min for a set of 5 samples. Resulting spectral data were analyzed using principal component analysis. The highest acetamiprid peak at 634 cm(-1) was used to detect and quantify the amount of acetamiprid spiked in 1:1 water-methanol solvent, apple juice, and on apple surface. The SERS method was able to successfully detect acetamiprid at 0.5 μg/mL (0.5 ppm) in solvent, 3 μg/mL (3 ppm) in apple juice, and 0.125 μg/cm(2) on apple surfaces. The SERS methods provide simple, rapid, and sensitive ways to detect acetamiprid in beverages and on the surfaces of thick skinned fruits and vegetables. © 2014 Institute of Food Technologists®

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.

Integrated microwave processing system for the extraction of organophosphorus pesticides in fresh vegetables.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-03-01

A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous pre-concentration and separation on simple paper-based analytical device for protein analysis.

PubMed

Niu, Ji-Cheng; Zhou, Ting; Niu, Li-Li; Xie, Zhen-Sheng; Fang, Fang; Yang, Fu-Quan; Wu, Zhi-Yong

2018-02-01

In this work, fast isoelectric focusing (IEF) was successfully implemented on an open paper fluidic channel for simultaneous concentration and separation of proteins from complex matrix. With this simple device, IEF can be finished in 10 min with a resolution of 0.03 pH units and concentration factor of 10, as estimated by color model proteins by smartphone-based colorimetric detection. Fast detection of albumin from human serum and glycated hemoglobin (HBA1c) from blood cell was demonstrated. In addition, off-line identification of the model proteins from the IEF fractions with matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was also shown. This PAD IEF is potentially useful either for point of care test (POCT) or biomarker analysis as a cost-effective sample pretreatment method.

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.

Determination of delorazepam in urine by solid-phase microextraction coupled to high performance liquid chromatography.

PubMed

Aresta, Antonella; Monaci, Linda; Zambonin, Carlo Giorgio

2002-06-01

An SPME-HPLC-UV method for the determination of delorazepam, a representative benzodiazepine, in spiked human urine samples was developed for the first time. The performances of two commercially available fibers, a carbowax/templated resin (Carbowax/TPR-100) and a polydimethylsiloxane/divinylbenzene (PDMS/DVB), were compared, indicating the latter as the most suitable for urine samples analysis. All the aspects influencing adsorption (extraction time, pH, temperature, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analyte on the fiber have been investigated. In particular, short extraction times were necessary to reach the equilibrium and very short desorption times were employed. The procedure required simple sample pre-treatment and was able to detect 5 ng/ml in spiked urine, regardless of the complexity of the matrix.

UV-Surface Treatment of Fungal Resistant Polyether Polyurethane Film-Induced Growth of Entomopathogenic Fungi

PubMed Central

Lando, Gabriela Albara; Marconatto, Letícia; Schrank, Augusto; Vainstein, Marilene Henning

2017-01-01

Synthetic polymers are the cause of some major environmental impacts due to their low degradation rates. Polyurethanes (PU) are widely used synthetic polymers, and their growing use in industry has produced an increase in plastic waste. A commercial polyether-based thermoplastic PU with hydrolytic stability and fungus resistance was only attacked by an entomopathogenic fungus, Metarhiziumanisopliae, when the films were pre-treated with Ultraviolet (UV) irradiation in the presence of reactive atmospheres. Water contact angle, Fourier transform infrared spectroscopy in attenuated total reflection mode (FTIR-ATR), scanning electron microscopy (SEM), and profilometer measurements were mainly used for analysis. Permanent hydrophilic PU films were produced by the UV-assisted treatments. Pristine polyether PU films incubated for 10, 30, and 60 days did not show any indication of fungal growth. On the contrary, when using oxygen in the UV pre-treatment a layer of fungi spores covered the sample, indicating a great adherence of the microorganisms to the polymer. However, if acrylic acid vapors were used during the UV pre-treatment, a visible attack by the entomopathogenic fungi was observed. SEM and FTIR-ATR data showed clear evidence of fungal development: growth and ramifications of hyphae on the polymer surface with the increase in UV pre-treatment time and fungus incubation time. The results indicated that the simple UV surface activation process has proven to be a promising alternative for polyether PU waste management. PMID:28718785

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.

Simultaneous determination of hydroquinone, resorcinol, phenol, m-cresol and p-cresol in untreated air samples using spectrofluorimetry and a custom multiple linear regression-successive projection algorithm.

PubMed

Pistonesi, Marcelo F; Di Nezio, María S; Centurión, María E; Lista, Adriana G; Fragoso, Wallace D; Pontes, Márcio J C; Araújo, Mário C U; Band, Beatriz S Fernández

2010-12-15

In this study, a novel, simple, and efficient spectrofluorimetric method to determine directly and simultaneously five phenolic compounds (hydroquinone, resorcinol, phenol, m-cresol and p-cresol) in air samples is presented. For this purpose, variable selection by the successive projections algorithm (SPA) is used in order to obtain simple multiple linear regression (MLR) models based on a small subset of wavelengths. For comparison, partial least square (PLS) regression is also employed in full-spectrum. The concentrations of the calibration matrix ranged from 0.02 to 0.2 mg L(-1) for hydroquinone, from 0.05 to 0.6 mg L(-1) for resorcinol, and from 0.05 to 0.4 mg L(-1) for phenol, m-cresol and p-cresol; incidentally, such ranges are in accordance with the Argentinean environmental legislation. To verify the accuracy of the proposed method a recovery study on real air samples of smoking environment was carried out with satisfactory results (94-104%). The advantage of the proposed method is that it requires only spectrofluorimetric measurements of samples and chemometric modeling for simultaneous determination of five phenols. With it, air is simply sampled and no pre-treatment sample is needed (i.e., separation steps and derivatization reagents are avoided) that means a great saving of time. Copyright © 2010 Elsevier B.V. All rights reserved.

Coupling of solvent-based de-emulsification dispersive liquid-liquid microextraction with high performance liquid chromatography for simultaneous simple and rapid trace monitoring of 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid.

PubMed

Behbahani, Mohammad; Najafi, Fatemeh; Bagheri, Saman; Bojdi, Majid Kalate; Hassanlou, Parmoon Ghareh; Bagheri, Akbar

2014-04-01

A simple, rapid, and efficient sample pretreatment technique, based on solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in water and urine samples. Some parameters such as acidity of solution, the amount of salt, type, and volume of extraction solvents, type of disperser/de-emulsifier solvent, and its volume were investigated and optimized. Under optimum extraction conditions, the limits of detections (LODs) of this method for MCPA and 2,4-D were 0.2 and 0.6 μg L(-1) (based on 3S(b)/m) in water and 0.4 and 1.6 μg L(-1) in urine, respectively. Furthermore, dynamic linear range of this method for MCPA and 2,4-D was 1-300 and 2-400 μg L(-1), repectively. Finally, the applicability of the proposed method was evaluated by extraction and determination of the herbicides in urine and different water samples.

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.

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.

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.

Rapid determination of caffeine in one drop of beverages and foods using drop-to-drop solvent microextraction with gas chromatography/mass spectrometry.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2007-11-02

A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis.

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.

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.

Online extraction-high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry for rapid flavonoid profiling of Fructus aurantii immaturus.

PubMed

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

2018-03-01

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 for Fructus aurantii immaturus (Zhishi), OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of eighteen flavonoids were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and compound 9, natsudaidain-3-O-glucoside, was discovered in Zhishi for the first time. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2018. Published by Elsevier B.V.

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.

Deficiency of cellulase activity measurements for enzyme evaluation.

PubMed

Pryor, Scott W; Nahar, Nurun

2010-11-01

Switchgrass was used as a model feedstock to determine the influence of pretreatment conditions and biomass quality on enzymatic hydrolysis using different enzyme products. Dilute sulfuric acid and soaking in aqueous ammonia pretreatments were used to produce biomass with varied levels of hemicellulose and lignin sheathing. Pretreated switchgrass solids were tested with simple enzymatic hydrolysis and simultaneous saccharification and fermentation (SSF) with three commercial enzyme products: Accellerase 1000 (Genencor), Spezyme CP (Genencor)/Novozyme 188 (Novozymes), and Celluclast/Novozyme 188 (Novozymes). Enzymes were loaded on a common activity basis (FPU/g cellulose and CBU/g cellulose). Despite identical enzyme loadings, glucose yields were significantly different for both acid and alkaline pretreatments but differences diminished as hydrolysis progressed for acid-pretreated biomass. Cellobiose concentrations in Accellerase treatments indicated an initial beta-glucosidase limitation that became less significant over time. SSF experiments showed that differences in glucose and ethanol yields could not be attributed to enzyme product inhibition. Yield discrepancies of glucose or ethanol in acid pretreatment, alkaline pretreatment, and acid pretreatment/SSF were as much as 15%, 19%, and 5%. These results indicate that standardized protocols for measuring enzyme activity may not be adequate for assessing activity using pretreated biomass substrates.

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.

Post-treatment mechanical refining as a method to improve overall sugar recovery of steam pretreated hybrid poplar.

PubMed

Dou, Chang; Ewanick, Shannon; Bura, Renata; Gustafson, Rick

2016-05-01

This study investigates the effect of mechanical refining to improve the sugar yield from biomass processed under a wide range of steam pretreatment conditions. Hybrid poplar chips were steam pretreated using six different conditions with or without SO2. The resulting water insoluble fractions were subjected to mechanical refining. After refining, poplar pretreated at 205°C for 10min without SO2 obtained a 32% improvement in enzymatic hydrolysis and achieved similar overall monomeric sugar recovery (539kg/tonne) to samples pretreated with SO2. Refining did not improve hydrolyzability of samples pretreated at more severe conditions, nor did it improve the overall sugar recovery. By maximizing overall sugar recovery, refining could partially decouple the pretreatment from other unit operations, and enable the use of low temperature, non-sulfur pretreatment conditions. The study demonstrates the possibility of using post-treatment refining to accommodate potential pretreatment process upsets without sacrificing sugar yields. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Determination of dimethyl fumarate in bakery food by d-SPE-HPLC-PDA].

PubMed

Yang, Jie; Luo, Mengtian; Feng, Di; Miao, Hong; Song, Shufeng; Zhao, Yunfeng

2015-05-01

To establish a simple and rapid pretreatment method with dispersive solid phase extraction ( d-SPE) by HPLC for determination of dimethyl fumarate in bakery foods. Dimethyl fumarate in samples was ultrasonically extracted by methanol, and cleaned up with d-SPE. Then, it was separated on C18 chromatographic column (4.6 mm x 25 mm, 5 μm) with a mixture of methanol--0.03 mol/L sodium acetate and 0.008 mol/L tetrabutyl ammonium bromide (40: 60, V/V) as mobile phase. The photodiode array detector was used in the determination under λ = 220 nm. In the linear range of 0.1 -25 μg/ml, the correlation coefficients was r > 0.999, and the average recoveries of the spiked samples were in the range of 82.8% - 107.5% with relative standard deviations (RSD) in the range of 3.30% - 7.30% (n = 6). The limit of detection ( LOD) was 0.4 mg/kg, and the limit of quantification was 1.0 mg/kg. The method is simple, rapid, sensitive and accurate, and suitable for determine dimethyl fumarate in bakery foods.

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.

[A simple and efficient method for establishing a mouse model of orthotopic MB49 bladder cancer].

PubMed

Liang, Zhong-kun; Zhang, Lin; Hu, Zhi-ming; Chen, Zhong; Huang, Xin; Shi, Xiang-hua; Tan, Wan-long; Gao, Ji-min

2009-04-01

To establish a simple and efficient method for establishing a mouse model of orthotopic superficial bladder cancer. C57BL/6 mice were anesthetized with sodium pentobarbital and catheterized with modified IV catheter (24 G). The mice were intravesically pretreated with HCl and then with NaOH, and after washing the bladders with phosphate-buffered saline (PBS), 100 microl (1 x 10(7)) MB49 cells were infused and allowed to incubate in the bladder for 2 h followed intravesical mitomycin C (MMC) administration. The tumor formation rate, survival, gross hematuria, and bladder weight were determined as the outcome variables, and the pathology of the bladders was observed. Instillation of MB49 tumor cells resulted in a tumor formation rates of 100% in all the pretreated groups while 0% in the control group without pretreatment. MMC significantly reduced the bladder weight as compared to PBS. We have successfully established a stable, reproducible, and reliable orthotopic bladder cancer model in mice.

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 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

Kinetic properties of Rhizopus oryzae RPG1 endo-polygalacturonase hydrolyzing galacturonic acid oligomers

USDA-ARS?s Scientific Manuscript database

Future fuel and specialty chemical production will benefit from the use of agricultural biomass. Efficient and effective use of agricultural biomass requires conversion to simple sugars by chemical pre-treatments and enzymes into simple sugars. Rhizopus oryzae, a filamentous fungus, makes enzymes ca...

The application of microwave digestion in decomposing some refractory ore samples with solid fusion agent.

PubMed

Lu, Yan; Li, Gang; Liu, Wei; Yuan, Hongyan; Xiao, Dan

2018-08-15

It is known that most of the refractory ore are the basis of national economy and widely applied in various fields, however, the complexity of the chemical composition and the diversity of the crystallinity in the mineral phases make the sample pre-treatment of refractory ore still remains a challenge. In this work, the complete decomposition of the refractory ore sample can be achieved just by exposing the solid fusion agent and the refractory ore sample in the microwave irradiation environment for a few minutes, and induced by a drop of water. A digestion time of 15 min for 3.0 g solid fusion agent mixture of sodium peroxide/sodium carbonate (Na 2 O 2 /Na 2 CO 3 ) in a corundum crucible via microwave heating is sufficient to decompose 0.1 g refractory ore sample. An excellent microwave digestion solid agent should meet the following conditions, a good decomposition ability, an outstanding ability of absorbing microwave energy and converting it into heat quickly, a higher melting point than the decomposing temperature of the ore sample. In the research, the induction effect of water plays an important role for the microwave digestion. The energy which is released by the reaction of water and the solid fusion agent (Na 2 O 2 ) is the key to decompose refractory ore samples with solid fusion agent, which replenished the total energy required for the microwave digestion and made the microwave digestion completed successfully. This microwave digestion technique has good reproducibility and precision, RSD % for Mo, Fe, Ti, Cr and W in the refractory ore samples were all better than 6, except RSD % for Be of about 8 because of the influence of matrix-effect. Meanwhile, the analysis results of the elements in the refractory ore samples provided by the microwave digestion technique were all in good agreement with the analysis results provided by the traditional fusion method except for Cr in the mixture ore samples. In the study, the non-linear dependence of the electromagnetic and thermal properties of the solid fusion agent on temperature under microwave irradiation and the selective heating of microwave are fully applied in this simple microwave technique. Comparing to the traditional fusion decomposition method, this microwave digestion technique is a simple, economical, fast and energy-saving sample pre-treatment technique. Copyright © 2018 Elsevier B.V. All rights reserved.

Detection of Soil Nitrogen Using Near Infrared Sensors Based on Soil Pretreatment and Algorithms

PubMed Central

Nie, Pengcheng; Dong, Tao; He, Yong; Qu, Fangfang

2017-01-01

Soil nitrogen content is one of the important growth nutrient parameters of crops. It is a prerequisite for scientific fertilization to accurately grasp soil nutrient information in precision agriculture. The information about nutrients such as nitrogen in the soil can be obtained quickly by using a near-infrared sensor. The data can be analyzed in the detection process, which is nondestructive and non-polluting. In order to investigate the effect of soil pretreatment on nitrogen content by near infrared sensor, 16 nitrogen concentrations were mixed with soil and the soil samples were divided into three groups with different pretreatment. The first group of soil samples with strict pretreatment were dried, ground, sieved and pressed. The second group of soil samples were dried and ground. The third group of soil samples were simply dried. Three linear different modeling methods are used to analyze the spectrum, including partial least squares (PLS), uninformative variable elimination (UVE), competitive adaptive reweighted algorithm (CARS). The model of nonlinear partial least squares which supports vector machine (LS-SVM) is also used to analyze the soil reflectance spectrum. The results show that the soil samples with strict pretreatment have the best accuracy in predicting nitrogen content by near-infrared sensor, and the pretreatment method is suitable for practical application. PMID:28492480

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.

Green coconut mesocarp pretreated by an alkaline process as raw material for bioethanol production.

PubMed

Soares, Jimmy; Demeke, Mekonnen M; Foulquié-Moreno, Maria R; Van de Velde, Miet; Verplaetse, Alex; Fernandes, Antonio Alberto Ribeiro; Thevelein, Johan M; Fernandes, Patricia Machado Bueno

2016-09-01

Cocos nucifera L., coconut, is a palm of high importance in the food industry, but a considerable part of the biomass is inedible. In this study, the pretreatment and saccharification parameters NaOH solution, pretreatment duration and enzyme load were evaluated for the production of hydrolysates from green coconut mesocarp using 18% (w/v) total solids (TS). Hydrolysates were not detoxified in order to preserve sugars solubilized during the pretreatment. Reduction of enzyme load from 15 to 7.5 filter paper cellulase unit (FPU)/g of biomass has little effect on the final ethanol titer. With optimized pretreatment and saccharification, hydrolysates with more than 7% (w/v) sugars were produced in 48h. Fermentation of the hydrolysate using industrial Saccharomyces cerevisiae strains produced 3.73% (v/v) ethanol. Our results showed a simple pretreatment condition with a high-solid load of biomass followed by saccharification and fermentation of undetoxified coconut mesocarp hydrolysates to produce ethanol with high titer. Copyright © 2016 Elsevier Ltd. All rights reserved.

[DNA quantification of blood samples pre-treated with pyramidon].

PubMed

Zhu, Chuan-Hong; Zheng, Dao-Li; Ni, Rao-Zhi; Wang, Hai-Sheng; Ning, Ping; Fang, Hui; Liu, Yan

2014-06-01

To study DNA quantification and STR typing of samples pre-treated with pyramidon. The blood samples of ten unrelated individuals were anticoagulated in EDTA. The blood stains were made on the filter paper. The experimental groups were divided into six groups in accordance with the storage time, 30 min, 1 h, 3 h, 6 h, 12 h and 24h after pre-treated with pyramidon. DNA was extracted by three methods: magnetic bead-based extraction, QIAcube DNA purification method and Chelex-100 method. The quantification of DNA was made by fluorescent quantitative PCR. STR typing was detected by PCR-STR fluorescent technology. In the same DNA extraction method, the sample DNA decreased gradually with times after pre-treatment with pyramidon. In the same storage time, the DNA quantification in different extraction methods had significant differences. Sixteen loci DNA typing were detected in 90.56% of samples. Pyramidon pre-treatment could cause DNA degradation, but effective STR typing can be achieved within 24 h. The magnetic bead-based extraction is the best method for STR profiling and DNA extraction.

Integrated microfluidic systems for cell lysis, mixing/pumping and DNA amplification

NASA Astrophysics Data System (ADS)

Lee, Chia-Yen; Lee, Gwo-Bin; Lin, Jr-Lung; Huang, Fu-Chun; Liao, Chia-Sheng

2005-06-01

The present paper reports a fully automated microfluidic system for the DNA amplification process by integrating an electroosmotic pump, an active micromixer and an on-chip temperature control system. In this DNA amplification process, the cell lysis is initially performed in a micro cell lysis reactor. Extracted DNA samples, primers and reagents are then driven electroosmotically into a mixing region where they are mixed by the active micromixer. The homogeneous mixture is then thermally cycled in a micro-PCR (polymerase chain reaction) chamber to perform DNA amplification. Experimental results show that the proposed device can successfully automate the sample pretreatment operation for DNA amplification, thereby delivering significant time and effort savings. The new microfluidic system, which facilitates cell lysis, sample driving/mixing and DNA amplification, could provide a significant contribution to ongoing efforts to miniaturize bio-analysis systems by utilizing a simple fabrication process and cheap materials.

Rapid screening of pharmaceutical drugs using thermal desorption - SALDI mass spectrometry

NASA Astrophysics Data System (ADS)

Grechnikov, A. A.; Kubasov, A. E.; Georgieva, V. B.; Borodkov, A. S.; Nikiforov, S. M.; Simanovsky, Ya O.; Alimpiev, S. S.

2012-12-01

A novel approach to the rapid screening of pharmaceutical drugs by surface assisted laser desorption-ionization (SALDI) mass spectrometry with the rotating ball interface coupled with temperature programmed thermal desorption has been developed. Analytes were thermally desorbed and deposited onto the surface of amorphous silicon substrate attached to the rotating ball. The ball was rotated and the deposited analytes were analyzed using SALDI. The effectiveness of coupling SALDI mass spectrometry with thermal desorption was evaluated by the direct and rapid analysis of tablets containing lidocaine, diphenhydramine and propranolol without any sample pretreatment. The overall duration of the screening procedure was 30÷40 sec. Real urine samples were studied for drug analysis. It is shown that with simple preparation steps, urine samples can be quantitatively analyzed using the proposed technique with the detection limits in the range of 0.2÷0.5 ng/ml.

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.

Two-stage dilute-acid and organic-solvent lignocellulosic pretreatment for enhanced bioprocessing.

PubMed

Brodeur, G; Telotte, J; Stickel, J J; Ramakrishnan, S

2016-11-01

A two stage pretreatment approach for biomass is developed in the current work in which dilute acid (DA) pretreatment is followed by a solvent based pretreatment (N-methyl morpholine N oxide - NMMO). When the combined pretreatment (DAWNT) is applied to sugarcane bagasse and corn stover, the rates of hydrolysis and overall yields (>90%) are seen to dramatically improve and under certain conditions 48h can be taken off the time of hydrolysis with the additional NMMO step to reach similar conversions. DAWNT shows a 2-fold increase in characteristic rates and also fractionates different components of biomass - DA treatment removes the hemicellulose while the remaining cellulose is broken down by enzymatic hydrolysis after NMMO treatment to simple sugars. The remaining residual solid is high purity lignin. Future work will focus on developing a full scale economic analysis of DAWNT for use in biomass fractionation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Two-stage dilute-acid and organic-solvent lignocellulosic pretreatment for enhanced bioprocessing

DOE PAGES

Brodeur, G.; Telotte, J.; Stickel, J. J.; ...

2016-08-26

A two stage pretreatment approach for biomass is developed in the current work in which dilute acid (DA) pretreatment is followed by a solvent based pretreatment (N-methyl morpholine N oxide -- NMMO). When the combined pretreatment (DAWNT) is applied to sugarcane bagasse and corn stover, the rates of hydrolysis and overall yields (>90%) are seen to dramatically improve and under certain conditions 48 h can be taken off the time of hydrolysis with the additional NMMO step to reach similar conversions. DAWNT shows a 2-fold increase in characteristic rates and also fractionates different components of biomass -- DA treatment removesmore » the hemicellulose while the remaining cellulose is broken down by enzymatic hydrolysis after NMMO treatment to simple sugars. The remaining residual solid is high purity lignin. Lastly, future work will focus on developing a full scale economic analysis of DAWNT for use in biomass fractionation.« less

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.

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.

Rapid-synthesis of zeolite T via sonochemical-assisted hydrothermal growth method.

PubMed

Jusoh, Norwahyu; Yeong, Yin Fong; Mohamad, Maisarah; Lau, Kok Keong; M Shariff, Azmi

2017-01-01

Sonochemical-assisted method has been identified as one of the potential pre-treatment methods which could reduce the formation duration of zeolite as well as other microporous and mesoporous materials. In the present work, zeolite T was synthesized via sonochemical-assisted pre-treatment prior to hydrothermal growth. The durations for sonochemical-assisted pre-treatment were varied from 30min to 90min. Meanwhile, the hydrothermal growth durations were ranged from 0.5 to 3days. The physicochemical properties of the resulting samples were characterized using XRD, FESEM, FTIR and BET. As verified by XRD, the samples synthesized via hydrothermal growth durations of 1, 2 and 3days and sonochemical-assisted pre-treatment durations of 60min and 90min demonstrated zeolite T structure. The samples which underwent sonochemical-assisted pre-treatment duration of 60min yielded higher crystallinity with negligible change of zeolite T morphology. Overall, the lengthy synthesis duration of zeolite T has been successfully reduced from 7days to 1day by applying sonochemical-assisted pre-treatment of 60min, while synthesis duration of 0.5days via sonochemical-assisted pre-treatment of 60min was not sufficient to produce zeolite T structure. Copyright © 2016 Elsevier B.V. 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.

Matrix-Assisted Plasma Atomization Emission Spectrometry for Surface Sampling Elemental Analysis

PubMed Central

Yuan, Xin; Zhan, Xuefang; Li, Xuemei; Zhao, Zhongjun; Duan, Yixiang

2016-01-01

An innovative technology has been developed involving a simple and sensitive optical spectrometric method termed matrix-assisted plasma atomization emission spectrometry (MAPAES) for surface sampling elemental analysis using a piece of filter paper (FP) for sample introduction. MAPAES was carried out by direct interaction of the plasma tail plume with the matrix surface. The FP absorbs energy from the plasma source and releases combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. The matrix-assisted plasma atomization excitation phenomenon was observed for multiple elements. The FP matrix served as the partial energy producer and also the sample substrate to adsorb sample solution. Qualitative and quantitative determinations of metal ions were achieved by atomic emission measurements for elements Ba, Cu, Eu, In, Mn, Ni, Rh and Y. The detection limits were down to pg level with linear correlation coefficients better than 0.99. The proposed MAPAES provides a new way for atomic spectrometry which offers advantages of fast analysis speed, little sample consumption, less sample pretreatment, small size, and cost-effective. PMID:26762972

Improved enzymatic hydrolysis of lignocellulosic biomass through pretreatment with plasma electrolysis.

PubMed

Gao, Jing; Chen, Li; Zhang, Jian; Yan, Zongcheng

2014-11-01

A comprehensive research on plasma electrolysis as pretreatment method for water hyacinth (WH) was performed based on lignin content, crystalline structure, surface property, and enzymatic hydrolysis. A large number of active particles, such as HO and H2O2, generated by plasma electrolysis could decompose the lignin of the biomass samples and reduce the crystalline index. An efficient pretreatment process made use of WH pretreated at a load of 48 wt% (0.15-0.18 mm) in FeCl3 solution for 30 min at 450 V. After the pretreatment, the sugar yield of WH was increased by 126.5% as compared with unpretreated samples. Copyright © 2014 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.

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.

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

Direct quantification of lipopeptide biosurfactants in biological samples via HPLC and UPLC-MS requires sample modification with an organic solvent.

PubMed

Biniarz, Piotr; Łukaszewicz, Marcin

2017-06-01

The rapid and accurate quantification of biosurfactants in biological samples is challenging. In contrast to the orcinol method for rhamnolipids, no simple biochemical method is available for the rapid quantification of lipopeptides. Various liquid chromatography (LC) methods are promising tools for relatively fast and exact quantification of lipopeptides. Here, we report strategies for the quantification of the lipopeptides pseudofactin and surfactin in bacterial cultures using different high- (HPLC) and ultra-performance liquid chromatography (UPLC) systems. We tested three strategies for sample pretreatment prior to LC analysis. In direct analysis (DA), bacterial cultures were injected directly and analyzed via LC. As a modification, we diluted the samples with methanol and detected an increase in lipopeptide recovery in the presence of methanol. Therefore, we suggest this simple modification as a tool for increasing the accuracy of LC methods. We also tested freeze-drying followed by solvent extraction (FDSE) as an alternative for the analysis of "heavy" samples. In FDSE, the bacterial cultures were freeze-dried, and the resulting powder was extracted with different solvents. Then, the organic extracts were analyzed via LC. Here, we determined the influence of the extracting solvent on lipopeptide recovery. HPLC methods allowed us to quantify pseudofactin and surfactin with run times of 15 and 20 min per sample, respectively, whereas UPLC quantification was as fast as 4 and 5.5 min per sample, respectively. Our methods provide highly accurate measurements and high recovery levels for lipopeptides. At the same time, UPLC-MS provides the possibility to identify lipopeptides and their structural isoforms.

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.

Coulometric sodium chloride removal system with Nafion membrane for seawater sample treatment.

PubMed

Grygolowicz-Pawlak, Ewa; Sohail, Manzar; Pawlak, Marcin; Neel, Bastien; Shvarev, Alexey; de Marco, Roland; Bakker, Eric

2012-07-17

Seawater analysis is one of the most challenging in the field of environmental monitoring, mainly due to disparate concentration levels between the analyte and the salt matrix causing interferences in a variety of analytical techniques. We propose here a miniature electrochemical sample pretreatment system for a rapid removal of NaCl utilizing the coaxial arrangement of an electrode and a tubular Nafion membrane. Upon electrolysis, chloride is deposited at the Ag electrode as AgCl and the sodium counterions are transported across the membrane. This cell was found to work efficiently at potentials higher than 400 mV in both stationary and flow injection mode. Substantial residual currents observed during electrolysis were found to be a result of NaCl back diffusion from the outer side of the membrane due to insufficient permselectivity of the Nafion membrane. It was demonstrated that the residual current can be significantly reduced by adjusting the concentration of the outer solution. On the basis of ion chromatography results, it was found that the designed cell used in flow injection electrolysis mode reduced the NaCl concentration from 0.6 M to 3 mM. This attempt is very important in view of nutrient analysis in seawater where NaCl is a major interfering agent. We demonstrate that the pretreatment of artificial seawater samples does not reduce the content of nitrite or nitrate ions upon electrolysis. A simple diffusion/extraction steady state model is proposed for the optimization of the electrolysis cell characteristics.

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

Optimization and validation of a fully automated silica-coated magnetic beads purification technology in forensics.

PubMed

Nagy, M; Otremba, P; Krüger, C; Bergner-Greiner, S; Anders, P; Henske, B; Prinz, M; Roewer, L

2005-08-11

Automated procedures for forensic DNA analyses are essential not only for large-throughput sample preparation, but are also needed to avoid errors during routine sample preparation. The most critical stage in PCR-based forensic analysis is DNA isolation, which should yield as much highly purified DNA as possible. The extraction method used consists of pre-treatment of stains and samples, cell lysis using chaotropic reagents, binding of the DNA to silica-coated magnetic particles, followed by elution of the DNA. Our work focuses mainly on sample preparation, obtaining the maximum possible amount of biological material from forensic samples, and the following cell lysis, to create a simple standardized lysis protocol suitable for nearly all forensic material. After optimization and validation, the M-48 BioRobot((R)) workstation has been used for more than 20,000 routine lab samples. There has been no evidence of cross contamination. Resulting DNA from as small as three nuclear cells yield reliable complete STR amplification profiles. The DNA remains stable after 2 years of storage.

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.

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.

Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

2018-03-01

A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Direct and quantitative analysis of underivatized acylcarnitines in serum and whole blood using paper spray mass spectrometry

PubMed Central

Yang, Qian; Manicke, Nicholas E.; Wang, He; Petucci, Christopher; Cooks, R. Graham

2013-01-01

A simple protocol for rapid quantitation of acylcarnitines in serum and whole blood has been developed using paper spray mass spectrometry. Dried serum and whole blood containing a mixture of ten acylcarnitines at various concentrations were analyzed as spots from paper directly without any sample pretreatment, separation, or derivatization. The composition of the spray solvent was found to be a critical factor: for serum samples, spray solvent of methanol/water/formic acid (80:20:0.1) gave the best signal intensity while for blood samples which contain more matrix components, acetonitrile/water (90:10) was a much more suitable spray solvent. For the paper type and size used, 0.5 μL of sample provided an optimal signal for both serum and whole blood samples. For quantitative profiling, the limits of quantitation obtained from both serum and blood were much lower than the clinically validated cutoff values for diagnosis of fatty acid oxidation disorders in newborn screening. Linearity (R2>0.95) and reproducibility (RSD ~10 %) were achieved in the concentration ranges from 100 nM to 5 μM for the C2 acylcarnitine, and for other acylcarnitines, these values were from 10 to 500 nM. Acylcarnitine profiles offer an effective demonstration of the fact that paper spray mass spectrometry is an appropriate, simple, rapid method with high sensitivity and high reproducibility applicable to newborn screening tests. PMID:22760507

Use of tannery wastewater as an alternative substrate and a pre-treatment medium for biogas production.

PubMed

Vazifehkhoran, Ali Heidarzadeh; Shin, Seung Gu; Triolo, Jin M

2018-06-01

This study investigated biogas production as an alternative treatment of tannery wastewater (TWW) and its use as a pre-treatment medium to increase CH 4 yield from anaerobic digestion (AD) of wheat straw. The TWW had high levels of sulfate and chloride, so biochemical CH 4 potential could be estimated only when the TWW was diluted. Untreated straw yielded 255 NL CH 4 (kg VS) -1 , whereas straw that had been pre-treated with TWW yielded 314 NL CH 4 (kg VS) -1 (35% increase). Treatment of TWW by AD with a co-substrate might be possible using a controlled feedstock mixing ratio. Use of TWW as a pre-treatment medium by simple co-storage before AD would be beneficial as an inexpensive treatment of lignocellulosic biomass. Copyright © 2018 Elsevier Ltd. All rights reserved.

Enhanced micropropagation and tiller formation in sugarcane through pretreatment of explants with thidiazuron (TDZ).

PubMed

Kumari, Kavita; Lal, Madan; Saxena, Sangeeta

2017-10-01

An efficient, simple and commercially applicable protocol for rapid micropropagation of sugarcane has been designed using variety Co 05011. Pretreatment of shoot tip explants with thidiazuron (TDZ) induced high frequency regeneration of shoot cultures with improved multiplication ratio. The highest frequency (80%) of shoot initiation in explants pretreated with 10 mg/l of TDZ was obtained during the study. Maximum 65% shoot cultures could be established from the explants pretreated with TDZ as compared to minimum 40% establishment in explants without pretreatment. The explants pretreated with 10 mg/l of TDZ required minimum 40 days for the establishment of shoot cultures as compared to untreated explants which required 60 days. The highest average number of shoots per culture (19.1) could be obtained from the explants pretreated with 10 mg/l of TDZ, indicating the highest multiplication ratio (1:6). Highest rooting (over 94%) was obtained in shoots regenerated from pretreated explants on ½ strength MS medium containing 5.0 mg/l of NAA and 50 g/l of sucrose within 15 days. Higher number of tillers/clump (15.3) could be counted in plants regenerated from pretreated explants than untreated ones (10.9 tillers/clump) in field condition, three months after transplantation. Molecular analysis using RAPD and DAMD markers suggested that the pretreatment of explants with TDZ did not adversely affect the genetic stability of regenerated plants and maintained high clonal purity.

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.

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.

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.

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

A gel-based visual immunoassay for non-instrumental detection of chloramphenicol in food samples.

PubMed

Yuan, Meng; Sheng, Wei; Zhang, Yan; Wang, Junping; Yang, Yijin; Zhang, Shuguang; Goryacheva, Irina Yu; Wang, Shuo

2012-11-02

A gel-based non-instrumental immuno-affinity assay was developed for the rapid screening of chloramphenicol (CAP) in food samples with the limit of detection (LOD) of 1 μg L(-1). The immuno-affinity test column (IATC) consisted of a test layer containing anti-CAP antibody coupled gel, and a control layer with anti-HRP antibody coupled gel. Based on the direct competitive immuno-reaction and the horseradish peroxidase enzymatic reaction, the test results could be evaluated visually. Basically, blue color development represented the negative results, while the absence of color development represented the positive results. In this study, CAP spiked samples of raw milk, pasteurized milk, UHT milk, skimmed milk powder, acacia honey, date honey, fish and shrimp were tested. Little or none sample pretreatment was required for this assay. The whole procedure was completed within 10min. In conclusion, the gel-based immuno-affinity test is a simple, rapid, and promising on-site screening method for CAP residues in food samples, with no instrumental requirement. Copyright © 2012 Elsevier B.V. All rights reserved.

Simple and sensitive analysis of blonanserin and blonanserin C in human plasma by liquid chromatography tandem mass spectrometry and its application.

PubMed

Zheng, Yunliang; Hu, Xingjiang; Liu, Jian; Wu, Guolan; Zhou, Huili; Zhu, Meixiang; Zhai, You; Wu, Lihua; Shentu, Jianzhong

2014-01-01

A highly sensitive, simple, and rapid liquid chromatography tandem mass spectrometry method to simultaneously determine blonanserin and blonanserin C in human plasma with AD-5332 as internal standard (IS) was established. A simple direct protein precipitation method was used for the sample pretreatment, and chromatographic separation was performed on a Waters XBridge C8 (4.6 × 150 mm, 3.5  μ m) column. The mobile phase consists of a mixture of 10 mM ammonium formate and 0.1% formic acid in water (A) and 0.1% formic acid in methanol (B). To quantify blonanserin, blonanserin C, and IS, multiple reaction monitoring (MRM) was performed in positive ESI mode. The calibration curve was linear in the concentration range of 0.012-5.78 ng·mL(-1) for blonanserin and 0.023-11.57 ng·mL(-1) for blonanserin C (r (2) > 0.9990). The intra- and interday precision of three quality control (QC) levels in plasma were less than 7.5%. Finally, the current simple, sensitive, and accurate LC-MS/MS method was successfully applied to investigate the pharmacokinetics of blonanserin and blonanserin C in healthy Chinese volunteers.

Simple and Sensitive Analysis of Blonanserin and Blonanserin C in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry and Its Application

PubMed Central

Zheng, Yunliang; Hu, Xingjiang; Liu, Jian; Wu, Guolan; Zhou, Huili; Zhu, Meixiang; Zhai, You; Wu, Lihua; ShenTu, Jianzhong

2014-01-01

A highly sensitive, simple, and rapid liquid chromatography tandem mass spectrometry method to simultaneously determine blonanserin and blonanserin C in human plasma with AD-5332 as internal standard (IS) was established. A simple direct protein precipitation method was used for the sample pretreatment, and chromatographic separation was performed on a Waters XBridge C8 (4.6 × 150 mm, 3.5 μm) column. The mobile phase consists of a mixture of 10 mM ammonium formate and 0.1% formic acid in water (A) and 0.1% formic acid in methanol (B). To quantify blonanserin, blonanserin C, and IS, multiple reaction monitoring (MRM) was performed in positive ESI mode. The calibration curve was linear in the concentration range of 0.012–5.78 ng·mL−1 for blonanserin and 0.023–11.57 ng·mL−1 for blonanserin C (r 2 > 0.9990). The intra- and interday precision of three quality control (QC) levels in plasma were less than 7.5%. Finally, the current simple, sensitive, and accurate LC-MS/MS method was successfully applied to investigate the pharmacokinetics of blonanserin and blonanserin C in healthy Chinese volunteers. PMID:24678425

Evaluation of constructed wetland treatment performance for winery wastewater.

PubMed

Grismer, Mark E; Carr, Melanie A; Shepherd, Heather L

2003-01-01

Rapid expansion of wineries in rural California during the past three decades has created contamination problems related to winery wastewater treatment and disposal; however, little information is available about performance of on-site treatment systems. Here, the project objective was to determine full-scale, subsurface-flow constructed wetland retention times and treatment performance through assessment of water quality by daily sampling of total dissolved solids, pH, total suspended solids, chemical oxygen demand (COD), tannins, nitrate, ammonium, total Kjeldahl nitrogen, phosphate, sulfate, and sulfide across operating systems for winery wastewater treatment. Measurements were conducted during both the fall crush season of heavy loading and the spring following bottling and racking operations at the winery. Simple decay model coefficients for these constituents as well as COD and tannin removal efficiencies from winery wastewater in bench-scale reactors are also determined. The bench-scale study used upward-flow, inoculated attached-growth (pea-gravel substrate) reactors fed synthetic winery wastewater. Inlet and outlet tracer studies for determination of actual retention times were essential to analyses of treatment performance from an operational subsurface-flow constructed wetland that had been overloaded due to failure to install a pretreatment system for suspended solids removal. Less intensive sampling conducted at a smaller operational winery wastewater constructed wetland that had used pretreatment suspended solids removal and aeration indicated that the constructed wetlands were capable of complete organic load removal from the winery wastewater.

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.

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.

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.

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.

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.

Ambient Ionization Mass Spectrometry Measurement of Aminotransferase Activity

NASA Astrophysics Data System (ADS)

Yan, Xin; Li, Xin; Zhang, Chengsen; Xu, Yang; Cooks, R. Graham

2017-06-01

A change in enzyme activity has been used as a clinical biomarker for diagnosis and is useful in evaluating patient prognosis. Current laboratory measurements of enzyme activity involve multi-step derivatization of the reaction products followed by quantitative analysis of these derivatives. This study simplified the reaction systems by using only the target enzymatic reaction and directly detecting its product. A protocol using paper spray mass spectrometry for identifying and quantifying the reaction product has been developed. Evaluation of the activity of aspartate aminotransferase (AST) was chosen as a proof-of-principle. The volume of sample needed is greatly reduced compared with the traditional method. Paper spray has a desalting effect that avoids sprayer clogging problems seen when examining serum samples by nanoESI. This very simple method does not require sample pretreatment and additional derivatization reactions, yet it gives high quality kinetic data, excellent limits of detection (60 ppb from serum), and coefficients of variation <10% in quantitation. [Figure not available: see fulltext.

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.

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.

Automated extraction of DNA from biological stains on fabric from crime cases. A comparison of a manual and three automated methods.

PubMed

Stangegaard, Michael; Hjort, Benjamin B; Hansen, Thomas N; Hoflund, Anders; Mogensen, Helle S; Hansen, Anders J; Morling, Niels

2013-05-01

The presence of PCR inhibitors in extracted DNA may interfere with the subsequent quantification and short tandem repeat (STR) reactions used in forensic genetic DNA typing. DNA extraction from fabric for forensic genetic purposes may be challenging due to the occasional presence of PCR inhibitors that may be co-extracted with the DNA. Using 120 forensic trace evidence samples consisting of various types of fabric, we compared three automated DNA extraction methods based on magnetic beads (PrepFiler Express Forensic DNA Extraction Kit on an AutoMate Express, QIAsyphony DNA Investigator kit either with the sample pre-treatment recommended by Qiagen or an in-house optimized sample pre-treatment on a QIAsymphony SP) and one manual method (Chelex) with the aim of reducing the amount of PCR inhibitors in the DNA extracts and increasing the proportion of reportable STR-profiles. A total of 480 samples were processed. The highest DNA recovery was obtained with the PrepFiler Express kit on an AutoMate Express while the lowest DNA recovery was obtained using a QIAsymphony SP with the sample pre-treatment recommended by Qiagen. Extraction using a QIAsymphony SP with the sample pre-treatment recommended by Qiagen resulted in the lowest percentage of PCR inhibition (0%) while extraction using manual Chelex resulted in the highest percentage of PCR inhibition (51%). The largest number of reportable STR-profiles was obtained with DNA from samples extracted with the PrepFiler Express kit (75%) while the lowest number was obtained with DNA from samples extracted using a QIAsymphony SP with the sample pre-treatment recommended by Qiagen (41%). Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

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.

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.

Paper-based assay for red blood cell antigen typing by the indirect antiglobulin test.

PubMed

Yeow, Natasha; McLiesh, Heather; Guan, Liyun; Shen, Wei; Garnier, Gil

2016-07-01

A rapid and simple paper-based elution assay for red blood cell antigen typing by the indirect antiglobulin test (IAT) was established. This allows to type blood using IgG antibodies for the important blood groups in which IgM antibodies do not exist. Red blood cells incubated with IgG anti-D were washed with saline and spotted onto the paper assay pre-treated with anti-IgG. The blood spot was eluted with an elution buffer solution in a chromatography tank. Positive samples were identified by the agglutinated and fixed red blood cells on the original spotting area, while red blood cells from negative samples completely eluted away from the spot of origin. Optimum concentrations for both anti-IgG and anti-D were identified to eliminate the washing step after the incubation phase. Based on the no-washing procedure, the critical variables were investigated to establish the optimal conditions for the paper-based assay. Two hundred ten donor blood samples were tested in optimal conditions for the paper test with anti-D and anti-Kell. Positive and negative samples were clearly distinguished. This assay opens up new applications of the IAT on paper including antibody detection and blood donor-recipient crossmatching and extends its uses into non-blood typing applications with IgG antibody-based diagnostics. Graphical abstract A rapid and simple paper-based assay for red blood cell antigen typing by the indirect antiglobulin test.

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.

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.

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.

Successive pretreatment and enzymatic saccharification of sugarcane bagasse in a packed bed flow-through column reactor aiming to support biorefineries.

PubMed

Terán-Hilares, R; Reséndiz, A L; Martínez, R T; Silva, S S; Santos, J C

2016-03-01

A packed bed flow-through column reactor (PBFTCR) was used for pretreatment and subsequent enzymatic hydrolysis of sugarcane bagasse (SCB). Alkaline pretreatment was performed at 70 °C for 4h with fresh 0.3M NaOH solution or with liquor recycled from a previous pretreatment batch. Scheffersomyces stipitis NRRL-Y7124 was used for fermentation of sugars released after enzymatic hydrolysis (20 FPU g(-1) of dry SCB). The highest results for lignin removal were 61% and 52%, respectively, observed when using fresh NaOH or the first reuse of the liquor. About 50% of cellulosic and 57% of hemicellulosic fractions of pretreated SCBs were enzymatically hydrolyzed and the maximum ethanol production was 23.4 g L(-1) (ethanol yield of 0.4 gp gs(-1)), with near complete consumption of both pentoses and hexoses present in the hydrolysate during the fermentation. PBFTCR as a new alternative for SCB-biorefineries is presented, mainly considering its simple configuration and efficiency for operating with a high solid:liquid ratio. Copyright © 2015 Elsevier Ltd. All rights reserved.

Hydrodynamic cavitation as a strategy to enhance the efficiency of lignocellulosic biomass pretreatment.

PubMed

Terán Hilares, Ruly; Ramos, Lucas; da Silva, Silvio Silvério; Dragone, Giuliano; Mussatto, Solange I; Santos, Júlio César Dos

2018-06-01

Hydrodynamic cavitation (HC) is a process technology with potential for application in different areas including environmental, food processing, and biofuels production. Although HC is an undesirable phenomenon for hydraulic equipment, the net energy released during this process is enough to accelerate certain chemical reactions. The application of cavitation energy to enhance the efficiency of lignocellulosic biomass pretreatment is an interesting strategy proposed for integration in biorefineries for the production of bio-based products. Moreover, the use of an HC-assisted process was demonstrated as an attractive alternative when compared to other conventional pretreatment technologies. This is not only due to high pretreatment efficiency resulting in high enzymatic digestibility of carbohydrate fraction, but also, by its high energy efficiency, simple configuration, and construction of systems, besides the possibility of using on the large scale. This paper gives an overview regarding HC technology and its potential for application on the pretreatment of lignocellulosic biomass. The parameters affecting this process and the perspectives for future developments in this area are also presented and discussed.

Modified graphene oxide sensors for ultra-sensitive detection of nitrate ions in water.

PubMed

Ren, Wen; Mura, Stefania; Irudayaraj, Joseph M K

2015-10-01

Nitrate ions is a very common contaminant in drinking water and has a significant impact on the environment, necessitating routine monitoring. Due to its chemical and physical properties, it is hard to directly detect nitrate ions with high sensitivity in a simple and inexpensive manner. Herein with amino group modified graphene oxide (GO) as a sensing element, we show a direct and ultra-sensitive method to detect nitrate ions, at a lowest detected concentration of 5 nM in river water samples, much lower than the reported methods based on absorption spectroscopy. Furthermore, unlike the reported strategies based on absorption spectroscopy wherein the nitrate concentration is determined by monitoring an increase in aggregation of gold nanoparticles (GNPs), our method evaluates the concentration of nitrate ions based on reduction in aggregation of GNPs for monitoring in real samples. To improve sensitivity, several optimizations were performed, including the assessment of the amount of modified GO required, concentration of GNPs and incubation time. The detection methodology was characterized by zeta potential, TEM and SEM. Our results indicate that an enrichment of modified GO with nitrate ions contributed to excellent sensitivity and the entire detection procedure could be completed within 75 min with only 20 μl of sample. This simple and rapid methodology was applied to monitor nitrate ions in real samples with excellent sensitivity and minimum pretreatment. The proposed approach paves the way for a novel means to detect anions in real samples and highlights the potential of GO based detection strategy for water quality monitoring. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Monitoring of Lactobacillus fermentation process by using ion chromatography with a series piezoelectric quartz crystal detector.

PubMed

Zhang, J; Xie, Y; Dai, X; Wei, W

2001-03-01

A new method monitoring Lactobacillus fermentation process, which combines ion chromatography (IC) with a series piezoelectric quartz crystal (SPQC) technique, is presented in this paper. Monitoring of the fermentation process was realized by examining the rate of production of lactic acid. An automatic membrane dialyser was used for the pretreatment of the sample in on-line monitoring. A mixture of p-hydroxybenzoic acid and N,N-diethylethanolamine was adopted as mobile phase and its flow rate was 0.8 ml/min. The effects of some fermentation conditions were also discussed in detail. Accordingly, the optimal fermentation conditions were obtained. This method is simple and convenient while the results obtained are accurate and reliable.

Biomass-water interactions correlate to recalcitrance and are intensified by pretreatment: An investigation of water constraint and retention in pretreated spruce using low field NMR and water retention value techniques.

PubMed

Weiss, Noah D; Thygesen, Lisbeth Garbrecht; Felby, Claus; Roslander, Christian; Gourlay, Keith

2017-01-01

The underlying mechanisms of the recalcitrance of biomass to enzymatic deconstruction are still not fully understood, and this hampers the development of biomass based fuels and chemicals. With water being necessary for most biological processes, it is suggested that interactions between water and biomass may be key to understanding and controlling biomass recalcitrance. This study investigates the correlation between biomass recalcitrance and the constraint and retention of water by the biomass, using SO 2 pretreated spruce, a common feedstock for lignocellulosic biofuel production, as a substrate to evaluate this relationship. The water retention value (WRV) of the pretreated materials was measured, and water constraint was assessed using time domain Low Field Nuclear Magnetic Resonance (LFNMR) relaxometry. WRV increased with pretreatment severity, correlating to reduced recalcitrance, as measured by hydrolysis of cellulose using commercial enzyme preparations. Water constraint increased with pretreatment severity, suggesting that a higher level of biomass-water interaction is indicative of reduced recalcitrance in pretreated materials. Both WRV and water constraint increased significantly with reductions in particle size when pretreated materials were further milled, suggesting that particle size plays an important role in biomass water interactions. It is suggested that WRV may be a simple and effective method for measuring and comparing biomass recalcitrance. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 33:146-153, 2017. © 2016 American Institute of Chemical Engineers.

Headspace-SPME-GC/MS as a simple cleanup tool for sensitive 2,6-diisopropylphenol analysis from lipid emulsions and adaptable to other matrices.

PubMed

Pickl, Karin E; Adamek, Viktor; Gorges, Roland; Sinner, Frank M

2011-07-15

Due to increased regulatory requirements, the interaction of active pharmaceutical ingredients with various surfaces and solutions during production and storage is gaining interest in the pharmaceutical research field, in particular with respect to development of new formulations, new packaging material and the evaluation of cleaning processes. Experimental adsorption/absorption studies as well as the study of cleaning processes require sophisticated analytical methods with high sensitivity for the drug of interest. In the case of 2,6-diisopropylphenol - a small lipophilic drug which is typically formulated as lipid emulsion for intravenous injection - a highly sensitive method in the concentration range of μg/l suitable to be applied to a variety of different sample matrices including lipid emulsions is needed. We hereby present a headspace-solid phase microextraction (HS-SPME) approach as a simple cleanup procedure for sensitive 2,6-diisopropylphenol quantification from diverse matrices choosing a lipid emulsion as the most challenging matrix with regard to complexity. By combining the simple and straight forward HS-SPME sample pretreatment with an optimized GC-MS quantification method a robust and sensitive method for 2,6-diisopropylphenol was developed. This method shows excellent sensitivity in the low μg/l concentration range (5-200μg/l), good accuracy (94.8-98.8%) and precision (intraday-precision 0.1-9.2%, inter-day precision 2.0-7.7%). The method can be easily adapted to other, less complex, matrices such as water or swab extracts. Hence, the presented method holds the potential to serve as a single and simple analytical procedure for 2,6-diisopropylphenol analysis in various types of samples such as required in, e.g. adsorption/absorption studies which typically deal with a variety of different surfaces (steel, plastic, glass, etc.) and solutions/matrices including lipid emulsions. Copyright © 2011 Elsevier B.V. All rights reserved.

A pretreatment method for HPLC analysis of cypermethrin in microbial degradation systems.

PubMed

Liu, Shuliang; Yao, Kai; Jia, Dongying; Zhao, Nan; Lai, Wen; Yuan, Huaiyu

2012-07-01

In this paper, a pretreatment method for high-performance liquid chromatography (HPLC) determination of cypermethrin (CY) in microbial degradation systems was systemically studied, primarily to solve the problem of inaccurate determination of CY concentration caused by its uneven distribution in the systems. A suitable pretreatment method was established, including sampling, extraction and dehydration of CY. Partial sampling could be taken for bacterial and yeast systems in which CY was uniformly dispersed by an emulsifying agent, while total sampling was only suitable for mold systems with or without an emulsifying agent. CY could be fully extracted from the samples in which microbial cells were disrupted by ultrasonic treatment with acetonitrile under ultrasonic condition. The extract could be effectively dehydrated and purified by passing it through an anhydrous Na(2)SO(4) column followed by an elution with acetonitrile. The determination of CY in the pretreated sample by HPLC showed a high precision [relative standard deviation (RSD) = 1.14%, n = 5] and a good stability over a period of five days (RSD = 1.57%, n = 5). The recoveries of CY in microbial degradation systems at three different spiked levels ranged from 95.68 to 108.09% (RSD = 0.50-5.87%, n = 5).

Use of Malachite Green-Loop Mediated Isothermal Amplification for Detection of Plasmodium spp. Parasites

PubMed Central

Lucchi, Naomi W.; Ljolje, Dragan; Silva-Flannery, Luciana; Udhayakumar, Venkatachalam

2016-01-01

Malaria elimination efforts are hampered by the lack of sensitive tools to detect infections with low-level parasitemia, usually below the threshold of standard diagnostic methods, microscopy and rapid diagnostic tests. Isothermal nucleic acid amplification assays such as the loop-mediated isothermal amplification (LAMP), are well suited for field use as they do not require thermal cyclers to run the test. However, the use of specialized equipment, as described by many groups, reduces the versatility of the LAMP technique as a simple tool for use in endemic countries. In this study, the use of the malachite green (MG) dye, as a visual endpoint readout, together with a simple mini heat block was evaluated for the detection of malaria parasites. The assay was performed for 1 hour at 63°C and the results scored by 3 independent human readers. The limit of detection of the assay was determined using well-quantified Plasmodium spp. infected reference samples and its utility in testing clinical samples was determined using 190 pre-treatment specimens submitted for reference diagnosis of imported malaria in the United States. Use of a simplified boil and spin methods of DNA extraction from whole blood and filter paper was also investigated. We demonstrate the accurate and sensitive detection of malaria parasites using this assay with a detection limit ranging between 1–8 parasites/μL, supporting its applicability for the detection of infections with low parasite burden. This assay is compatible with the use of a simple boil and spin sample preparation method from both whole blood and filter papers without a loss of sensitivity. The MG-LAMP assay described here has great potential to extend the reach of molecular tools to settings where they are needed. PMID:26967908

Rapid, in situ detection of cocaine residues based on paper spray ionization coupled with ion mobility spectrometry.

PubMed

Li, Ming; Zhang, Jingjing; Jiang, Jie; Zhang, Jing; Gao, Jing; Qiao, Xiaolin

2014-04-07

In this paper, a novel approach based on paper spray ionization coupled with ion mobility spectrometry (PSI-IMS) was developed for rapid, in situ detection of cocaine residues in liquid samples and on various surfaces (e.g. glass, marble, skin, wood, fingernails), without tedious sample pretreatment. The obvious advantages of PSI are its low cost, easy operation and simple configuration without using nebulizing gas or discharge gas. Compared with mass spectrometry, ion mobility spectrometry (IMS) takes advantage of its low cost, easy operation, and simple configuration without requiring a vacuum system. Therefore, IMS is a more congruous detection method for PSI in the case of rapid, in situ analysis. For the analysis of cocaine residues in liquid samples, dynamic responses from 5 μg mL(-1) to 200 μg mL(-1) with a linear coefficient (R(2)) of 0.992 were obtained. In this case, the limit of detection (LOD) was calculated to be 2 μg mL(-1) as signal to noise (S/N) was 3 with a relative standard deviation (RSD) of 6.5% for 11 measurements (n = 11). Cocaine residues on various surfaces such as metal, glass, marble, wood, skin, and fingernails were also directly analyzed before wiping the surfaces with a piece of paper. The LOD was calculated to be as low as 5 ng (S/N = 3, RSD = 6.3%, n = 11). This demonstrates the capability of the PSI-IMS method for direct detection of cocaine residues at scenes of cocaine administration. Our results show that PSI-IMS is a simple, sensitive, rapid and economical method for in situ detection of this illicit drug, which could help governments to combat drug abuse.

Evaluations of cellulose accessibilities of lignocelluloses by solute exclusion and protein adsorption techniques

Treesearch

Q.Q. Wang; Z. He; Z. Zhu; Y.-H.P. Zhang; Y. Ni; X.L. Luo; J.Y. Zhu

2012-01-01

Cellulose accessibilities of a set of hornified lignocellulosic substrates derived by drying the never dried pretreated sample and a set of differently pretreated lodgepople pine substrates, were evaluated using solute exclusion and protein adsorption methods. Direct measurements of cellulase adsorption onto cellulose surface of the set of pretreated substrates were...

Effects of enzyme loading and β-glucosidase supplementation on enzymatic hydrolysis of switchgrass processed by leading pretreatment technologies.

PubMed

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; Donohoe, Bryon S; Vinzant, Todd B; Elander, Richard T; Hames, Bonnie; Thomas, Steve; Warner, Ryan E

2011-12-01

The objective of this work is to investigate the effects of cellulase loading and β-glucosidase supplementation on enzymatic hydrolysis of pretreated Dacotah switchgrass. To assess the difference among various pretreatment methods, the profiles of sugars and intermediates were determined for differently treated substrates. For all pretreatments, 72 h glucan/xylan digestibilities increased sharply with enzyme loading up to 25mg protein/g-glucan, after which the response varied depending on the pretreatment method. For a fixed level of enzyme loading, dilute sulfuric acid (DA), SO(2), and Lime pretreatments exhibited higher digestibility than the soaking in aqueous ammonia (SAA) and ammonia fiber expansion (AFEX). Supplementation of Novozyme-188 to Spezyme-CP improved the 72 h glucan digestibility only for the SAA treated samples. The effect of β-glucosidase supplementation was discernible only at the early phase of hydrolysis where accumulation of cellobiose and oligomers is significant. Addition of β-glucosidase increased the xylan digestibility of alkaline treated samples due to the β-xylosidase activity present in Novozyme-188. Copyright © 2011 Elsevier Ltd. All rights reserved.

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.

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.

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.

Quantitation of polyamines in cultured cells and tissue homogenates by reversed-phase high-performance liquid chromatography of their benzoyl derivatives.

PubMed

Verkoelen, C F; Romijn, J C; Schroeder, F H; van Schalkwijk, W P; Splinter, T A

1988-04-08

A rapid and simple method, originally described by Redmond and Tseng [J. Chromatogr., 170 (1979) 479] was applied to the analysis of di- and polyamines in cultured human tumour cells and human tumour xenografts. Optimization of the procedures and evaluation of the characteristic features of the assay are described. The (modified) procedure employs precolumn derivatization with benzoyl chloride, extraction of the derivatives by chloroform, separation by reversed-phase high-performance liquid chromatography under isocratic conditions and detection by ultraviolet absorbance measurement at 229 nm. The complete analysis was accomplished within 10 min per sample. The detection limit was ca. 1 pmol. The intra- and inter-assay coefficients of variation were 2.5-4.4% and 3.4-13.1%, respectively. The presence of well known inhibitors of polyamine biosynthesis, such as DL-alpha-difluoromethylornithine and methylglyoxal bis(guanylhydrazone), did not interfere with the assay, and disturbance by cyclohexylamine could be avoided by changing the polarity of the mobile phase. The method proved to be very suitable because it is rapid, simple, requires a minimum of sample pretreatment, and still provides sufficient sensitivity to quantitate polyamines in relatively small amounts of cells (10(5) cells) or tumour tissues (less than 1 mg), even after treatment with inhibitors of polyamine biosynthesis.

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.

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.

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

Mobility of arsenic and its compounds in soil and soil solution: the effect of soil pretreatment and extraction methods.

PubMed

Száková, J; Tlustos, P; Goessler, W; Frková, Z; Najmanová, J

2009-12-30

The effect of soil extraction procedures and/or sample pretreatment (drying, freezing of the soil sample) on the extractability of arsenic and its compounds was tested. In the first part, five extraction procedures were compared with following order of extractable arsenic portions: 2M HNO(3)>0.43 M CH(3)COOH>or=0.05 M EDTA>or=Mehlich III (0.2M CH(3)COOH+0.25 M NH(4)NO(3)+0.013 M HNO(3)+0.015 M NH(4)F+0.001 M EDTA) extraction>water). Additionally, two methods of soil solution sampling were compared, centrifugation of saturated soil and the use of suction cups. The results showed that different sample pretreatments including soil solution sampling could lead to different absolute values of mobile arsenic content in soils. However, the interpretation of the data can lead to similar conclusions as apparent from the comparison of the soil solution sampling methods (r=0.79). For determination of arsenic compounds mild extraction procedures (0.05 M (NH(4))(2)SO(4), 0.01 M CaCl(2), and water) and soil solution sampling using suction cups were compared. Regarding the real soil conditions the extraction of fresh samples and/or in situ collection of soil solution are preferred among the sample pretreatments and/or soil extraction procedures. However, chemical stabilization of the solutions should be allowed and included in the analytical procedures for determination of individual arsenic compounds.

Removal of Water-Soluble Extractives Improves the Enzymatic Digestibility of Steam-Pretreated Softwood Barks.

PubMed

Frankó, Balázs; Carlqvist, Karin; Galbe, Mats; Lidén, Gunnar; Wallberg, Ola

2018-02-01

Softwood bark contains a large amounts of extractives-i.e., soluble lipophilic (such as resin acids) and hydrophilic components (phenolic compounds, stilbenes). The effects of the partial removal of water-soluble extractives before acid-catalyzed steam pretreatment on enzymatic digestibility were assessed for two softwood barks-Norway spruce and Scots pine. A simple hot water extraction step removed more than half of the water-soluble extractives from the barks, which improved the enzymatic digestibility of both steam-pretreated materials. This effect was more pronounced for the spruce than the pine bark, as evidenced by the 30 and 11% glucose yield improvement, respectively, in the enzymatic digestibility. Furthermore, analysis of the chemical composition showed that the acid-insoluble lignin content of the pretreated materials decreased when water-soluble extractives were removed prior to steam pretreatment. This can be explained by a decreased formation of water-insoluble "pseudo-lignin" from water-soluble bark phenolics during the acid-catalyzed pretreatment, which otherwise results in distorted lignin analysis and may also contribute to the impaired enzymatic digestibility of the barks. Thus, this study advocates the removal of extractives as the first step in the processing of bark or bark-rich materials in a sugar platform biorefinery.

Microfluidic thread based electroanalytical system for green chromatographic separations.

PubMed

Agustini, Deonir; Fedalto, Lucas; Bergamini, Márcio F; Marcolino-Junior, Luiz Humberto

2018-02-13

The use of miniaturized chromatographic systems is an important strategy for reducing the consumption of supplies related to separations, allowing the development of more sustainable analytical methodologies. However, the high cost and complexity in the production of these systems combined with the operational difficulties and the need for the use of solvent and sample pretreatment are challenges to be overcome in order to make the chromatographic methods greener. Here, we report the construction and development of a low cost microfluidic system for green and solvent-free chromatographic separations with electrochemical detection integrated into cotton threads without the use of any mechanical pumping to transport the solutions. The manufacture of the proposed system was performed by simple assembly of the components, with the separation of the species based on an ion exchange mechanism and detection using gold electrodes manufactured directly on the cotton threads. A linear range of 0.025-5.0 mM was obtained for the effective separation of ascorbic acid (AA) and dopamine (DA) with detection limits of 2.89 μM (for AA) and 4.41 μM (for DA). Each analysis was performed at a low cost (less than 0.01 dollars), and with a small volume of waste generated (107.1 μL). So, the proposed system was successfully employed to determine the levels of AA and DA present in the tears of healthy volunteers without sample pretreatment, indicating the good analytical performance of the system and the possibility of performing greener chromatographic separations.

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.

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

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.

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...

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.

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

Preliminary study of an exercise programme for reducing fatigue and improving sleep among long-term haemodialysis patients.

PubMed

Maniam, Radha; Subramanian, Pathmawathi; Singh, Surindar Kaur Surat; Lim, Soo Kun; Chinna, Karuthan; Rosli, Roshaslina

2014-09-01

Fatigue and quality of sleep are the main factors that contribute to a poor quality of life among patients on long-term haemodialysis. Studies have also emphasised the importance of exercise for improving the wellbeing of dialysis patients. This study aimed to determine the effectiveness of a predialysis low-to-moderate-intensity exercise programme for reducing fatigue and improving sleep disorders among long-term haemodialysis patients. In this quasi-experimental study, an exercise programme was conducted three times a week for 12 weeks before long-term haemodialysis patients underwent dialysis at two centres. The patients were categorised into either the exercise group (n = 28) or control group (n = 27). The latter was asked to maintain their current lifestyles. Assessments of fatigue and sleep disorder levels were performed for both groups using self-reported questionnaires at baseline and after intervention. The patients' perception of the exercise programme was also determined using self-reported questionnaires. Paired sample t-test indicated improvements in fatigue level in the exercise group (mean fatigue score: post-treatment 40.5 ± 7.9 vs. pre-treatment 30.0 ± 10.9). Improvements in sleep disorders were also observed in the exercise group (mean score: post-treatment 7.6 ± 3.3 vs. pre-treatment 10.1 ± 3.8). However, sleep quality deteriorated in the control group (mean score: post-treatment 10.7 ± 2.9 vs. pre-treatment 9.3 ± 2.9). Simple low-to-moderate-intensity exercise is effective for improving fatigue, sleep disorders and the overall quality of life among haemodialysis patients.

[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.

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.

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.

Dissolution of Lignocelluloses with a High Lignin Content in a N-Methylmorpholine-N-oxide Monohydrate Solvent System via Simple Glycerol-Swelling and Mechanical Pretreatments.

PubMed

Zhang, Lili; Lu, Hailong; Yu, Juan; Wang, Zhiguo; Fan, Yimin; Zhou, Xiaofan

2017-11-08

Lignocelluloses (LCs) with various amounts of lignin (even as high as 18.4%) were successfully dissolved in N-methylmorpholine-N-oxide monohydrate (NMMO/H 2 O) solution with stirring at 85 °C within 5 h. For the developmental dissolution methods of LCs with a high lignin content in NMMO/H 2 O solution, the following two pretreatment steps of LCs were necessary: (1) glycerol swelling and (2) mechanical extrusion. The mechanical extrusion pretreatment under glycerol swelling dissociated the fiber bundles of LCs to thinner fibers and, thus, enhanced the accessibility and solubility of the LCs in NMMO/H 2 O. The crystal structure of the pretreated LCs had no significant transformation during pretreatment, while the diameters of the fiber bundles were reduced from 50-60 to 10-12 μm, as investigated by X-ray diffraction and scanning electron microscopy. After the dissolution-regeneration process of LCs, the fiber bundles of the LCs disappeared and the crystal type of cellulose in the LCs was transformed from cellulose I to cellulose II, which indicated the complete dissolution of LCs.

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.

Simple column-switching ion chromatography method for determining eight monosaccharides and oligosaccharides in honeydew and nectar.

PubMed

Ni, Chengzhu; Zhu, Binhe; Wang, Nani; Wang, Muhua; Chen, Suqing; Zhang, Jiajie; Zhu, Yan

2016-03-01

Honeydew is excreted by aphids as a sweet waste and nectar is floral honey. Honeydew and nectar are complicated samples which consist of various sugars and amino acids. In this work, a simple ion chromatography with column-switching method was developed for the simultaneous analysis of 8 monosaccharides and oligosaccharides in honeydew and nectar. A reversed-phase column was used as a pretreatment column to eliminate organics on-line and sugars were eluted from a collection loop to analytical column by using column-switching technique. This method showed good linearity (r⩾0.9994) and afforded low limits of detection ranging from 1.55 to 10.17μgL(-1) for all the analytes. Recoveries ranged from 95% to 105% and repeatability results were acceptable with relative standard deviation of less than 3.21% (n=6). This method was successfully applied to quantification of these sugars in honeydew and nectar. These results showed honeydew had much more oligosaccharides than nectar. Copyright © 2015 Elsevier Ltd. All rights reserved.

A simple and cost-effective method, as an appropriate alternative for visible spectrophotometry: development of a dopamine biosensor.

PubMed

Abbaspour, Abdolkarim; Khajehzadeh, Abdolreza; Ghaffarinejad, Ali

2009-08-01

In this study, a new, simple, fast and inexpensive method as an alternative to visible spectrophotometry is developed. In this method the cells containing the sample solution were scanned with a scanner, then the color of each cell was analyzed with software written in visual basic (VB 6) media to red, green and blue values. The cells were built by creating holes in the Plexiglas sheet. The dimensions of identical cells were examined by Cr (III) solution with known concentrations. The validity of this new method was studied by determination of dopamine (DA) without using any other reagent. The parameters which affect the system were optimized. The comparison between the current and traditional UV-Vis spectrophotometry methods was studied and the results revealed similar trends in both methods. The developed method was successfully applied to the determination of dopamine in serum and urine without using any pretreatment. Finally comparing the results obtained in the developed method showed that microwave irradiation of the solution can decrease the experimental time, increase sensitivity and improve the limit of detection.

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.

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.

[Determination of biphenyl ether herbicides in water using HPLC with cloud-point extraction].

PubMed

He, Cheng-Yan; Li, Yuan-Qian; Wang, Shen-Jiao; Ouyang, Hua-Xue; Zheng, Bo

2010-01-01

To determine residues of multiple biphenyl ether herbicides simultaneously in water using high performance liquid chromatography (HPLC) with cloud-point extraction. The residues of eight biphenyl ether herbicides (including bentazone, fomesafen, acifluorfen, aclonifen, bifenox, fluoroglycofenethy, nitrofen, oxyfluorfen) in water samples were extracted with cloud-point extraction of Triton X-114. The analytes were separated and determined using reverse phase HPLC with ultraviolet detector at 300 nm. Optimized conditions for the pretreatment of water samples and the parameters of chromatographic separation applied. There was a good linear correlation between the concentration and the peak area of the analytes in the range of 0.05-2.00 mg/L (r = 0.9991-0.9998). Except bentazone, the spiked recoveries of the biphenyl ether herbicides in the water samples ranged from 80.1% to 100.9%, with relative standard deviations ranging from 2.70% to 6.40%. The detection limit of the method ranged from 0.10 microg/L to 0.50 microg/L. The proposed method is simple, rapid and sensitive, and can meet the requirements of determination of multiple biphenyl ether herbicides simultaneously in natural waters.

Simultaneous quantification of reparixin and paclitaxel in plasma and urine using ultra performance liquid chromatography-tandem mass spectroscopy (UHPLC-MS/MS): Application to a preclinical pharmacokinetic study in rats.

PubMed

Malhi, Sarandeep; Stesco, Nicholas; Alrushaid, Samaa; Lakowski, Ted M; Davies, Neal M; Gu, Xiaochen

2017-03-01

A liquid chromatography-tandem mass spectroscopy (LC-MS/MS) assay was developed and validated to simultaneously quantify anticancer drugs reparixin and paclitaxel in this study. The compounds were extracted from plasma and urine samples by protein precipitation with acetone (supplemented with 0.1% formic acid). Chromatographic separation was achieved using a C18 column, and drug molecules were ionized using dual ion source electrospray and atmospheric pressure chemical ionization (DUIS: ESI-APCI). Reparixin and paclitaxel were quantified using negative and positive multiple reaction monitoring (MRM) mode, respectively. Stable isotope palcitaxel-D5 was used as the internal standard (IS). The assay was validated for specificity, recovery, carryover and sample stability under various storage conditions; it was also successfully applied to measure drug concentrations collected from a pharmacokinetic study in rats. The results confirmed that the assay was accurate and simple in quantifying both reparixin and paclitaxel in plasma and urine with minimal sample pretreatment. Copyright © 2016 Elsevier B.V. All rights reserved.

A new approach for bisphenol A detection employing fluorosurfactant-capped gold nanoparticle-amplified chemiluminescence from cobalt(II) and peroxymonocarbonate.

PubMed

Pan, Feng; Liu, Lin; Dong, Shichao; Lu, Chao

2014-07-15

In this work, we utilized the nonionic fluorosurfactant-capped gold nanoparticles (GNPs) as a novel chemiluminescence (CL) probe for the determination of trace bisphenol A. Bisphenol A can induce a sharp decrease in CL intensity from the GNP-Co(2+)-peroxymonocarbonate (HCO4(-)) system. Under the selected experimental conditions, a linear relationship was obtained between the CL intensity and the logarithm of concentration of bisphenol A in the range of 0.05-50 μM (R(2) = 0.9936), and the detection limit at a signal-to-noise ratio of 3 for bisphenol A was 10 nM. The applicability of the proposed method has been validated by determining bisphenol A in real polycarbonate samples with satisfactory results. The recoveries for bisphenol A in spiked samples were found to be between 94.4% and 105.0%. The relative standard deviation (RSD) for 12 repeated measurements of 0.5 μM bisphenol A was 2.2%. The proposed method described herein was simple, selective and obviated the need of extensive sample pretreatment. Copyright © 2014 Elsevier B.V. All rights reserved.

LC-MS based analysis of endogenous steroid hormones in human hair.

PubMed

Gao, Wei; Kirschbaum, Clemens; Grass, Juliane; Stalder, Tobias

2016-09-01

The quantification of endogenous steroid hormone concentrations in hair is increasingly used as a method for obtaining retrospective information on long-term integrated hormone exposure. Several different analytical procedures have been employed for hair steroid analysis, with liquid chromatography-mass spectrometry (LC-MS) being recognized as a particularly powerful analytical tool. Several methodological aspects affect the performance of LC-MS systems for hair steroid analysis, including sample preparation and pretreatment, steroid extraction, post-incubation purification, LC methodology, ionization techniques and MS specifications. Here, we critically review the differential value of such protocol variants for hair steroid hormones analysis, focusing on both analytical quality and practical feasibility issues. Our results show that, when methodological challenges are adequately addressed, LC-MS protocols can not only yield excellent sensitivity and specificity but are also characterized by relatively simple sample processing and short run times. This makes LC-MS based hair steroid protocols particularly suitable as a high-quality option for routine application in research contexts requiring the processing of larger numbers of samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Validation and Clinical Evaluation of a Novel Method To Measure Miltefosine in Leishmaniasis Patients Using Dried Blood Spot Sample Collection

PubMed Central

Rosing, H.; Hillebrand, M. J. X.; Blesson, S.; Mengesha, B.; Diro, E.; Hailu, A.; Schellens, J. H. M.; Beijnen, J. H.

2016-01-01

To facilitate future pharmacokinetic studies of combination treatments against leishmaniasis in remote regions in which the disease is endemic, a simple cheap sampling method is required for miltefosine quantification. The aims of this study were to validate a liquid chromatography-tandem mass spectrometry method to quantify miltefosine in dried blood spot (DBS) samples and to validate its use with Ethiopian patients with visceral leishmaniasis (VL). Since hematocrit (Ht) levels are typically severely decreased in VL patients, returning to normal during treatment, the method was evaluated over a range of clinically relevant Ht values. Miltefosine was extracted from DBS samples using a simple method of pretreatment with methanol, resulting in >97% recovery. The method was validated over a calibration range of 10 to 2,000 ng/ml, and accuracy and precision were within ±11.2% and ≤7.0% (≤19.1% at the lower limit of quantification), respectively. The method was accurate and precise for blood spot volumes between 10 and 30 μl and for Ht levels of 20 to 35%, although a linear effect of Ht levels on miltefosine quantification was observed in the bioanalytical validation. DBS samples were stable for at least 162 days at 37°C. Clinical validation of the method using paired DBS and plasma samples from 16 VL patients showed a median observed DBS/plasma miltefosine concentration ratio of 0.99, with good correlation (Pearson's r = 0.946). Correcting for patient-specific Ht levels did not further improve the concordance between the sampling methods. This successfully validated method to quantify miltefosine in DBS samples was demonstrated to be a valid and practical alternative to venous blood sampling that can be applied in future miltefosine pharmacokinetic studies with leishmaniasis patients, without Ht correction. PMID:26787691

Trace elements determination in seawater by ICP-MS with on-line pre-concentration on a Chelex-100 column using a ‘standard’ instrument setup.

PubMed Central

Søndergaard, Jens; Asmund, Gert; Larsen, Martin M.

2015-01-01

Trace element determination in seawater is analytically challenging due to the typically very low concentrations of the trace elements and the potential interference of the salt matrix. A common way to address the challenge is to pre-concentrate the trace elements on a chelating resin, then rinse the matrix elements from the resin and subsequently elute and detect the trace elements using inductively coupled plasma mass spectrometry (ICP-MS). This technique typically involves time-consuming pre-treatment of the samples for ‘off-line’ analyses or complicated sample introduction systems involving several pumps and valves for ‘on-line’ analyses. As an alternative, the following method offers a simple method for ‘on-line’ analyses of seawater by ICP-MS. As opposed to previous methods, excess seawater was pumped through the nebulizer of the ICP-MS during the pre-concentration step but the gas flow was adjusted so that the seawater was pumped out as waste without being sprayed into the instrument. Advantages of the method include: • Simple and convenient analyses of seawater requiring no changes to the ‘standard’ sample introduction system except from a resin-filled micro-column connected to the sample tube. The ‘standard’ sample introduction system refers to that used for routine digest-solution analyses of biota and sediment by ICP-MS using only one peristaltic pump; and • Accurate determination of the elements V, Mn, Co, Ni, Cu, Zn, Cd and Pb in a range of different seawater matrices verified by participation in 6 successive rounds of the international laboratory intercalibration program QUASIMEME. PMID:26258050

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.

Determination of microstickies in recycled whitewater by headspace gas chromatography.

PubMed

Chai, X-S; Samp, J C; Yang, Q F; Song, H N; Zhang, D C; Zhu, J Y

2006-03-03

This study proposed a novel headspace gas chromatographic (HS-GC) method for determination of adhesive contaminants (microstickies) in recycled whitewater, a fiber containing process stream, in the paper mill. It is based on the adsorption behavior of toluene (as a tracer) on the hydrophobic surface of microstickies, which affects the apparent vapor-liquid equilibration partitioning of toluene. It was found that the equilibrium concentration of toluene in the vapor phase is inversely proportional to the apparent effective surface area of microstickies that remain in the corresponding solution. Thus, the amount of microsticky materials in the recycled whitewater can be quantified by HS-GC via indirect measurement of the toluene content in the vapor phase of the sample without any pretreatment. The presented method is simple, rapid and automated.

HPLC determination of four active saponins from Panax notoginseng in rat serum and its application to pharmacokinetic studies.

PubMed

Li, Lie; Sheng, Yuxin; Zhang, Jinlan; Wang, Chuanshe; Guo, Dean

2004-12-01

Four main active saponins (ginsenosides Rg1, Rb1, Rd and notoginsenoside R1) in Panax notoginseng in rat serum after oral and intravenous administration of total saponins of P. notoginseng (PNS) to rats were determined using a simple and sensitive high-performance chromatographic method. The serum samples were pretreated with solid-phase extraction before analysis. The calibration curves for the four saponins were linear in the given concentration ranges. The intra-day and inter-day assay coefficients in serum were less than 10.0% and the recoveries of the method were higher than 80.0% in the high, middle and low concentrations. This method was applied to study the pharmacokinetics following oral and intravenous administration of PNS. Copyright 2004 John Wiley & Sons, Ltd.

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.

SiC Nanowires Synthesized by Rapidly Heating a Mixture of SiO and Arc-Discharge Plasma Pretreated Carbon Black.

PubMed

Wang, Feng-Lei; Zhang, Li-Ying; Zhang, Ya-Fei

2008-11-22

SiC nanowires have been synthesized at 1,600 degrees C by using a simple and low-cost method in a high-frequency induction furnace. The commercial SiO powder and the arc-discharge plasma pretreated carbon black were mixed and used as the source materials. The heating-up and reaction time is less than half an hour. It was found that most of the nanowires have core-shell SiC/SiO(2) nanostructures. The nucleation, precipitation, and growth processes were discussed in terms of the oxide-assisted cluster-solid mechanism.

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.

Direct and sensitive detection of foodborne pathogens within fresh produce samples using a field-deployable handheld device.

PubMed

You, David J; Geshell, Kenneth J; Yoon, Jeong-Yeol

2011-10-15

Direct and sensitive detection of foodborne pathogens from fresh produce samples was accomplished using a handheld lab-on-a-chip device, requiring little to no sample processing and enrichment steps for a near-real-time detection and truly field-deployable device. The detection of Escherichia coli K12 and O157:H7 in iceberg lettuce was achieved utilizing optimized Mie light scatter parameters with a latex particle immunoagglutination assay. The system exhibited good sensitivity, with a limit of detection of 10 CFU mL(-1) and an assay time of <6 min. Minimal pretreatment with no detrimental effects on assay sensitivity and reproducibility was accomplished with a simple and cost-effective KimWipes filter and disposable syringe. Mie simulations were used to determine the optimal parameters (particle size d, wavelength λ, and scatter angle θ) for the assay that maximize light scatter intensity of agglutinated latex microparticles and minimize light scatter intensity of the tissue fragments of iceberg lettuce, which were experimentally validated. This introduces a powerful method for detecting foodborne pathogens in fresh produce and other potential sample matrices. The integration of a multi-channel microfluidic chip allowed for differential detection of the agglutinated particles in the presence of the antigen, revealing a true field-deployable detection system with decreased assay time and improved robustness over comparable benchtop systems. Additionally, two sample preparation methods were evaluated through simulated field studies based on overall sensitivity, protocol complexity, and assay time. Preparation of the plant tissue sample by grinding resulted in a two-fold improvement in scatter intensity over washing, accompanied with a significant increase in assay time: ∼5 min (grinding) versus ∼1 min (washing). Specificity studies demonstrated binding of E. coli O157:H7 EDL933 to only O157:H7 antibody conjugated particles, with no cross-reactivity to K12. This suggests the adaptability of the system for use with a wide variety of pathogens, and the potential to detect in a variety of biological matrices with little to no sample pretreatment. Copyright © 2011 Elsevier B.V. All rights reserved.

Study on the autofluorescence profiles of iris pigment epithelium and retinal pigment epithetlium

NASA Astrophysics Data System (ADS)

Xu, Gaixia; Qu, Junle; Chen, Danni; Sun, Yiwen; Zhao, Lingling; Lin, Ziyang; Ding, Zhihua; Niu, Hanben

2007-05-01

Transplantation technique of retinal pigment epithelium has been noticeable in recent years and gradually put into clinical practice in treatment of retinal degenerative diseases. Generally, immunological, histochemical, and physical methods are used to study the iris pigment epithelium (IPE) and retinal pigment epithelium (RPE) cells, which need complex sample preparation. In this paper, we provided a simple autofluorescence microscopy to investigate the fresh porcine IPE and RPE cells without any pretreatment. The results showed that the morphology and size of both were similar, round and about 15 μm. The main flourophore in both cells was similar, i.e. lipofuscin. In additional, the autofluorescence spectrum of RPE shifted blue after light-induced damage by laser illuminating. Because it was easier for IPE to be damaged by laser than for RPE, and the power of one scanning operation to get a full image was strong enough to damage IPE sample, we hadn't get any satisfied autofluorescence spectrum of IPE.

Rapid Analysis of Bisphenol A and Its Analogues in Food Packaging Products by Paper Spray Ionization Mass Spectrometry.

PubMed

Chen, Shuo; Chang, Quanying; Yin, Kai; He, Qunying; Deng, Yongxiu; Chen, Bo; Liu, Chengbin; Wang, Ying; Wang, Liping

2017-06-14

In this study, a paper spray ionization mass spectrometric (PS-MS) method was developed for the rapid in situ screening and simultaneous quantitative analysis of bisphenol A and its analogues, i.e., bisphenol S, bisphenol F, and bisphenol AF, in food packaging products. At the optimal PS-MS conditions, the calibration curves of bisphenols in the range of 1-100 μg/mL were linear. The correlation coefficients were higher than 0.998, and the LODs of the target compounds were 0.1-0.3 μg/mL. After a simple treatment by dichloromethane on the surface, the samples were analyzed by PS-MS in situ for rapid screening without a traditional sample pretreatment procedure, such as powdering, extraction, and enrichment steps. The analytical time of the PS-MS method was less than 1 min. In comparison with conventional HPLC-MS/MS, it was demonstrated that PS-MS was a more effective high-throughput screening and quantitative analysis method.

Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon)

PubMed Central

Ledesma-Escobar, Carlos A.; Priego-Capote, Feliciano; Luque de Castro, María D.

2016-01-01

Background Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far. Objective Evaluate the effect of both the sample pretreatment and the extraction method on the profile of flavonoids isolated from lemon. Results Extracts from fresh, lyophilized and air-dried samples obtained by shaking extraction (SE), ultrasound-assisted extraction (USAE), microwave-assisted extraction (MAE) and superheated liquid extraction (SHLE) were analyzed by LC–QTOF MS/MS, and 32 flavonoids were tentatively identified using MS/MS information. ANOVA applied to the data from fresh and dehydrated samples and from extraction by the different methods revealed that 26 and 32 flavonoids, respectively, were significant (p≤0.01). The pairwise comparison (Tukey HSD; p≤0.01) showed that lyophilized samples are more different from fresh samples than from air-dried samples; also, principal component analysis (PCA) showed a clear discrimination among sample pretreatment strategies and suggested that such differences are mainly created by the abundance of major flavonoids. On the other hand, pairwise comparison of extraction methods revealed that USAE and MAE provided quite similar extracts, being SHLE extracts different from the other two. In this case, PCA showed a clear discrimination among extraction methods, and their position in the scores plot suggests a lower abundance of flavonoids in the extracts from SHLE. In the two PCA the loadings plots revealed a trend to forming groups according to flavonoid aglycones. Conclusions The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied conditions, liophilization provides extracts with higher amounts of flavonoids, and USAE is the best method for isolation of these compounds, followed by MAE and SE. On the contrary, the SHLE method was the less favorable to extract flavonoids from citrus owing to degradation. PMID:26807979

Ambient air levels and health risk assessment of benzo(a)pyrene in atmospheric particulate matter samples from low-polluted areas: application of an optimized microwave extraction and HPLC-FL methodology.

PubMed

de la Gala Morales, María; Holgado, Fernando Rueda; Marín, Ma Rosario Palomo; Blázquez, Lorenzo Calvo; Gil, Eduardo Pinilla

2015-04-01

A new methodology involving a simple and fast pretreatment of the samples by microwave-assisted extraction and concentration by N2 stream, followed by HPLC with fluorescence detection, was used for determining the concentration of benzo(a)pyrene (BaP) in atmospheric particulate matter (PM10 fraction). Obtained LOD, 1.0 × 10(-3) ng/m(3), was adequate for the analysis of benzo(a)pyrene in the samples, and BaP recovery from PAH in Fine Dust (PM10-like) certified reference material was nearly quantitative (86%). The validated procedure was applied for analyzing 115 PM10 samples collected at different sampling locations in the low-polluted area of Extremadura (Southwest Spain) during a monitoring campaign carried out in 2011-2012. BaP spatial variations and seasonal variability were investigated as well as the influence of meteorological conditions and different air pollutants concentrations. A normalized protocol for health risk assessment was applied to estimate lifetime cancer risk due to BaP inhalation in the sampling areas, finding that around eight inhabitants per million people may develop lung cancer due to the exposition to BaP in atmospheric particulates emitted by the investigated sources.

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.

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.

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

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.

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.

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.

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites.

PubMed

Xie, Li; Chen, Liqin; Gu, Pan; Wei, Lanlan; Kang, Xuejun

2018-03-01

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and related diseases, but their precise measurement is still a challenge. Many protocols have been described for neurotransmitter measurement by a variety of instruments, including high-pressure liquid chromatography (HPLC). However, there are shortcomings, such as complicated operation or hard-to-detect multiple targets, which cannot be avoided, and presently, the dominant analysis technique is still HPLC coupled with sensitive electrochemical or fluorimetric detection, due to its high sensitivity and good selectivity. Here, a detailed protocol is described for the pretreatment and detection of catecholamines with high pressure liquid chromatography with electrochemical detection (HPLC-ECD) in real urine samples of infants, using electrospun composite nanofibers composed of polymeric crown ether with polystyrene as adsorbent, also known as the packed-fiber solid phase extraction (PFSPE) method. We show how urine samples can be easily precleaned by a nanofiber-packed solid phase column, and how the analytes in the sample can be rapidly enriched, desorbed, and detected on an ECD system. PFSPE greatly simplifies the pretreatment procedures for biological samples, allowing for decreased time, expense, and reduction of the loss of targets. Overall, this work illustrates a simple and convenient protocol for solid-phase extraction coupled to an HPLC-ECD system for simultaneous determination of three monoamine neurotransmitters (norepinephrine (NE), epinephrine (E), dopamine (DA)) and two of their metabolites (3-methoxy-4-hydroxyphenylglycol (MHPG) and 3,4-dihydroxy-phenylacetic acid (DOPAC)) in infants' urine. The established protocol was applied to assess the differences of urinary catecholamines and their metabolites between high-risk infants with perinatal brain damage and healthy controls. Comparative analysis revealed a significant difference in urinary MHPG between the two groups, indicating that the catecholamine metabolites may be an important candidate marker for early diagnosis of cases at risk for brain damage in infants.

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.

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.

Enhanced enzymatic saccharification of corn stover by in situ modification of lignin with poly (ethylene glycol) ether during low temperature alkali pretreatment.

PubMed

Lai, Chenhuan; Tang, Shuo; Yang, Bo; Gao, Ziqi; Li, Xin; Yong, Qiang

2017-11-01

A novel pretreatment process of corn stover was established in this study by in situ modification of lignin with poly (ethylene glycol) diglycidyl ether (PEGDE) during low temperature alkali pretreatment. The addition of PEGDE obviously improved the enzymatic hydrolysis by covalently modifying the residual lignins in substrates. Under the optimized conditions (pretreated with 10% (w/w) NaOH and 10% (w/w) PEGDE at 70°C for 2.5h), the total fermentable sugar yield was increased by 46.4%, from 23.7g to 34.7g per 100g raw materials. Additionally, the remaining activities of exo-glucanase and β-glucosidase in supernatant were increased by 58.6% and 40.6% respectively, demonstrating that the enhancement of enzymatic hydrolysis was mainly due to the alleviation of enzyme non-productive binding. Although the isolated lignin modified with PEGDE enhanced the enzymatic hydrolysis of substrates as well, this in situ lignin modification provided an efficient but simple way to improve enzymatic saccharification. Copyright © 2017. Published by Elsevier Ltd.

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.

Direct detection of hyaluronidase in urine using cationic gold nanoparticles: a potential diagnostic test for bladder cancer.

PubMed

Nossier, Ahmed Ibrahim; Eissa, Sanaa; Ismail, Manal Fouad; Hamdy, Mohamed Ahmed; Azzazy, Hassan Mohamed El-Said

2014-04-15

Hyaluronidase (HAase) was reported as a urinary marker of bladder cancer. In this study, a simple colorimetric gold nanoparticle (AuNP) assay was developed for rapid and sensitive detection of urinary HAase activity. Charge interaction between polyanionic hyaluronic acid (HA) and cationic AuNPs stabilized with cetyl trimethyl ammonium bromide (CTAB) led to formation of gold aggregates and a red to blue color shift. HAase digests HA into small fragments preventing the aggregation of cationic AuNPs. The nonspecific aggregation of AuNPs in urine samples was overcome by pre-treatment of samples with the polycationic chitosan that was able to agglomerate all negatively charged interfering moieties before performing the assay. The developed AuNP assay was compared with zymography for qualitative detection of urinary HAase activity in 40 bladder carcinoma patients, 11 benign bladder lesions patients and 15 normal individuals, the assay sensitivity was 82.5% vs. 65% for zymography, while the specificity for both assays was 96.1%. The absorption ratio, A530/A620 of the reacted AuNP solution was used to quantify the HAase activity. The best cut off value was 93.5 μU/ng protein, at which the sensitivity was 90% and the specificity was 80.8%.The developed colorimetric AuNP HAase assay is simple, inexpensive, and can aid noninvasive diagnosis of bladder cancer. © 2013 Elsevier B.V. All rights reserved.

A new chiral residue analysis method for triazole fungicides in water using dispersive liquid-liquid microextraction (DLLME).

PubMed

Luo, Mai; Liu, Donghui; Zhou, Zhiqiang; Wang, Peng

2013-09-01

A rapid, simple, reliable, and environment-friendly method for the residue analysis of the enantiomers of four chiral fungicides including hexaconazole, triadimefon, tebuconazole, and penconazole in water samples was developed by dispersive liquid-liquid microextraction (DLLME) pretreatment followed by chiral high-performance liquid chromatography (HPLC)-DAD detection. The enantiomers were separated on a Chiralpak IC column by HPLC applying n-hexane or petroleum ether as mobile phase and ethanol or isopropanol as modifier. The influences of mobile phase composition and temperature on the resolution were investigated and most of the enantiomers could be completely separated in 20 min under optimized conditions. The thermodynamic parameters indicated that the separation was enthalpy-driven. The elution orders were detected by both circular dichroism detector (CD) and optical rotatory dispersion detector (ORD). Parameters affecting the DLLME performance for pretreatment of the chiral fungicides residue in water samples, such as the extraction and dispersive solvents and their volume, were studied and optimized. Under the optimum microextraction condition the enrichment factors were over 121 and the linearities were 30-1500 µg L(-1) with the correlation coefficients (R(2)) over 0.9988 and the recoveries were between 88.7% and 103.7% at the spiking levels of 0.5, 0.25, and 0.05 mg L(-1) (for each enantiomer) with relative standard deviations varying from 1.38% to 6.70% (n = 6) The limits of detection (LODs) ranged from 8.5 to 29.0 µg L(-1) (S/N = 3). © 2013 Wiley Periodicals, Inc.

[Rapid fabrication of molecularly imprinted polymer fibers for solid phase microextraction of bisphenol A].

PubMed

Hu, Mei; Zhang, Yijun; Yang, Jinghua; Zhou, Xiaomao; Wei, Zhuqing; Ding, Xiaoqing; Zhang, Yuping

2015-02-01

The rapid preparation of molecularly imprinted polymer (MIP) fibers was reported using bisphenol A (BPA) as the template molecular, acetonitrile (ACN) as the porogenic solvent, α-methacrylic acid (MAA) as the functional monomer, ethylene dimethacrylate (EDMA) as the crosslinker, and azodiisobutyronitrile (AIBN) as the thermal initiator. It was carried out within a capillary of 530 µm inner diameter (I. D.) by microwave irradiation in 7 min. The resulted BPA-MIP fibers were pushed out from the capillary, eluted in a vial and inserted in the capillary again followed by the application of the solid phase microextraction (SPME) procedure. The extraction performance was investigated in detail by varying the molar ratios between the template and the monomer (BPA/MAA), the concentration of NaCl, the extraction and desorption time, the pH value and the desorption solvents. The selectivity of the prepared MIP and non-molecularly imprinted polymer (NIP) fibers was comparatively evaluated by selecting two structurally-related compounds, phenol (P) and 4-phenylphenol (PP), and non-analogue dicyandiamide (DCD). The established method was successfully applied for the pretreatment and determination of BPA from beverage samples coupled to high performance liquid chromatography (HPLC). Under the optimal conditions, the linear range of BPA was 10-400 µg/L; the detection limit (LOD) was 0.45 µg/L and the recoveries spiked in the mineral water were 88.4%-102. 8%. The results demonstrated that the developed method can determine BPA in real samples with some advantages of simple pretreatment, rapid analysis, low limit of detection and low consumption of materials.

Germination and soil seed bank traits of Podocarpus angustifolius (Podocarpaceae): an endemic tree species from Cuban rain forests.

PubMed

Ferrandis, Pablo; Bonilla, Marta; Osorio, Licet del Carmen

2011-09-01

Podocarpus angustifolius is an endangered recalcitrant-seeded small tree, endemic to mountain rain forests in the central and Pinar del Río regions in Cuba. In this study, the germination patterns of P. angustifolius seeds were evaluated and the nature of the soil seed bank was determined. Using a weighted two-factor design, we analyzed the combined germination response to seed source (i.e. freshly matured seeds directly collected from trees versus seeds extracted from soil samples) and pretreatment (i.e. seed water-immersion for 48h at room temperature). Germination was delayed for four weeks (= 30 days) in all cases, regardless of both factors analyzed. Moreover, nine additional days were necessary to achieve high germination values (in the case of fresh, pretreated seeds). These results overall may indicate the existence of a non-deep simple morphophysiological dormancy in P. angustifolius seeds. The water-immersion significantly enhanced seed germination, probably as a result of the hydration of recalcitrant seeds. Although germination of seeds extracted from soil samples was low, probably due to aging and pathogen effects throughout the time of burial, the study revealed the existence of a persistent soil seed bank (at least short-termed) of approximately 42 viable seeds per m2 in the upper 10cm of soil. Such a record is noteworthy since references to persistent soil seed banks in recalcitrant-seeded species are scarce in the literature. The population consequences derived from the formation of persistent soil seed banks in this endangered species are discussed.

Hydrothermal pretreatment of several lignocellulosic mixtures containing wheat straw and two hardwood residues available in Southern Europe.

PubMed

Silva-Fernandes, Talita; Duarte, Luís Chorão; Carvalheiro, Florbela; Loureiro-Dias, Maria Conceição; Fonseca, César; Gírio, Francisco

2015-05-01

This work studied the processing of biomass mixtures containing three lignocellulosic materials largely available in Southern Europe, eucalyptus residues (ER), wheat straw (WS) and olive tree pruning (OP). The mixtures were chemically characterized, and their pretreatment, by autohydrolysis, evaluated within a severity factor (logR0) ranging from 1.73 up to 4.24. A simple modeling strategy was used to optimize the autohydrolysis conditions based on the chemical characterization of the liquid fraction. The solid fraction was characterized to quantify the polysaccharide and lignin content. The pretreatment conditions for maximal saccharides recovery in the liquid fraction were at a severity range (logR0) of 3.65-3.72, independently of the mixture tested, which suggests that autohydrolysis can effectively process mixtures of lignocellulosic materials for further biochemical conversion processes. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

Biobutanol production from apple pomace: the importance of pretreatment methods on the fermentability of lignocellulosic agro-food wastes.

PubMed

Hijosa-Valsero, María; Paniagua-García, Ana I; Díez-Antolínez, Rebeca

2017-11-01

Apple pomace was studied as a possible raw material for biobutanol production. Five different soft physicochemical pretreatments (autohydrolysis, acids, alkalis, organic solvents and surfactants) were compared in a high-pressure reactor, whose working parameters (temperature, time and reagent concentration) were optimised to maximise the amount of simple sugars released and to minimise inhibitor generation. The pretreated biomass was subsequently subjected to a conventional enzymatic treatment to complete the hydrolysis. A thermal analysis (DSC) of the solid biomass indicated that lignin was mainly degraded during the enzymatic treatment. The hydrolysate obtained with the surfactant polyethylene glycol 6000 (PEG 6000) (1.96% w/w) contained less inhibitors than any other pretreatment, yet providing 42 g/L sugars at relatively mild conditions (100 °C, 5 min), and was readily fermented by Clostridium beijerinckii CECT 508 in 96 h (3.55 g/L acetone, 9.11 g/L butanol, 0.26 g/L ethanol; 0.276 g B /g S yield; 91% sugar consumption). Therefore, it is possible to optimise pretreatment conditions of lignocellulosic apple pomace to reduce inhibitor concentrations in the final hydrolysate and perform successful ABE fermentations without the need of a detoxification stage.

A sensitive chemiluminescence enzyme immunoassay based on molecularly imprinted polymers solid-phase extraction of parathion.

PubMed

Chen, Ge; Jin, Maojun; Du, Pengfei; Zhang, Chan; Cui, Xueyan; Zhang, Yudan; She, Yongxin; Shao, Hua; Jin, Fen; Wang, Shanshan; Zheng, Lufei; Wang, Jing

2017-08-01

The chemiluminescence enzyme immunoassay (CLEIA) method responds differently to various sample matrices because of the matrix effect. In this work, the CLEIA method was coupled with molecularly imprinted polymers (MIPs) synthesized by precipitation polymerization to study the matrix effect. The sample recoveries ranged from 72.62% to 121.89%, with a relative standard deviation (RSD) of 3.74-18.14%.The ratio of the sample matrix-matched standard curve slope rate to the solvent standard curve slope was 1.21, 1.12, 1.17, and 0.85 for apple, rice, orange and cabbage in samples pretreated with the mixture of PSA and C 18 . However, the ratio of sample (apple, rice, orange, and cabbage) matrix-matched standard-MIPs curve slope rate to the solvent standard curve was 1.05, 0.92, 1.09, and 1.05 in samples pretreated with MIPs, respectively. The results demonstrated that the matrices of the samples greatly interfered with the detection of parathion residues by CLEIA. The MIPs bound specifically to the parathion in the samples and eliminated the matrix interference effect. Therefore, the CLEIA method have successfully applied MIPs in sample pretreatment to eliminate matrix interference effects and provided a new sensitive assay for agro-products. Copyright © 2017 Elsevier Inc. All rights reserved.

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.

Simultaneous determination of eleven preservatives in cosmetics by micellar electrokinetic chromatography.

PubMed

Wang, Ping; Ding, Xiaojing; Li, Yun; Yang, Yuanyuan

2012-01-01

A new method for the simultaneous quantitation of 11 preservatives-imidazolidinyl urea, benzyl alcohol, dehydroacetic acid, sorbic acid, phenoxyethanol, benzoic acid, salicylic acid, and four parabens (methyl, ethyl, propyl, and butyl)-in cosmetics by micellar electrokinetic capillary chromatography was established and validated. The separation was performed using an uncoated fused-silica capillary (50 pm id x 60.2 cm, effective length 50 cm) with a running buffer consisting of 15 mmol/L sodium tetraborate, 60 mmol/L boric acid, and 100 mmol/L sodium dodecyl sulfate. A 1:10 dilution of the running buffer was used as the sample buffer to extract the cosmetic samples. The key factors, such as the concentration and pH of the running and sample buffers, which influence quantitative analysis of the above 11 preservatives in cosmetic samples, were investigated in detail. The linear ranges of the calibration curves for imidazolidinyl urea and the other 10 preservatives were 50-1000 and 10-200 mg/L, respectively. The correlation coefficients of the standard curves were all higher than 0.999. The recoveries at the concentrations studied ranged from 93.0 to 102.7%. RSDs were all less than 5%. The new method with simple sample pretreatment met the needs for routine analysis of the 11 preservatives in cosmetics.

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.

Preliminary study of an exercise programme for reducing fatigue and improving sleep among long-term haemodialysis patients

PubMed Central

Maniam, Radha; Subramanian, Pathmawathi; Singh, Surindar Kaur Surat; Lim, Soo Kun; Chinna, Karuthan; Rosli, Roshaslina

2014-01-01

INTRODUCTION Fatigue and quality of sleep are the main factors that contribute to a poor quality of life among patients on long-term haemodialysis. Studies have also emphasised the importance of exercise for improving the wellbeing of dialysis patients. This study aimed to determine the effectiveness of a predialysis low-to-moderate-intensity exercise programme for reducing fatigue and improving sleep disorders among long-term haemodialysis patients. METHODS In this quasi-experimental study, an exercise programme was conducted three times a week for 12 weeks before long-term haemodialysis patients underwent dialysis at two centres. The patients were categorised into either the exercise group (n = 28) or control group (n = 27). The latter was asked to maintain their current lifestyles. Assessments of fatigue and sleep disorder levels were performed for both groups using self-reported questionnaires at baseline and after intervention. The patients’ perception of the exercise programme was also determined using self-reported questionnaires. RESULTS Paired sample t-test indicated improvements in fatigue level in the exercise group (mean fatigue score: post-treatment 40.5 ± 7.9 vs. pre-treatment 30.0 ± 10.9). Improvements in sleep disorders were also observed in the exercise group (mean score: post-treatment 7.6 ± 3.3 vs. pre-treatment 10.1 ± 3.8). However, sleep quality deteriorated in the control group (mean score: post-treatment 10.7 ± 2.9 vs. pre-treatment 9.3 ± 2.9). CONCLUSION Simple low-to-moderate-intensity exercise is effective for improving fatigue, sleep disorders and the overall quality of life among haemodialysis patients. PMID:25273932

Effectiveness of saliva and fingerprints as alternative specimens to urine and blood in forensic drug testing.

PubMed

Kuwayama, Kenji; Miyaguchi, Hajime; Yamamuro, Tadashi; Tsujikawa, Kenji; Kanamori, Tatsuyuki; Iwata, Yuko T; Inoue, Hiroyuki

2016-07-01

In forensic drug testing, it is important to immediately take biological specimens from suspects and victims to prove their drug intake. We evaluated the effectiveness of saliva and fingerprints as alternative specimens to urine and blood in terms of ease of sampling, drug detection sensitivity, and drug detection periods for each specimen type. After four commercially available pharmaceutical products were administered to healthy subjects, each in a single dose, their urine, blood, saliva, and fingerprints were taken at predetermined sampling times over approximately four weeks. Fourteen analytes (the administered drugs and their main metabolites) were extracted from each specimen using simple pretreatments, such as dilution and deproteinization, and were analyzed using liquid chromatography/mass spectrometry (LC/MS). Most of the analytes were detected in saliva and fingerprints, as well as in urine and blood. The time-courses of drug concentrations were similar between urine and fingerprints, and between blood and saliva. Compared to the other compounds, the acidic compounds, for example ibuprofen, acetylsalicylic acid, were more difficult to detect in all specimens. Acetaminophen, dihydrocodeine, and methylephedrine were detected in fingerprints at later sampling times than in urine. However, a relationship between the drug structures and their detection periods in each specimen was not found. Saliva and fingerprints could be easily sampled on site without using special techniques or facilities. In addition, fingerprints could be immediately analyzed after simple and rapid treatment. In cases where it would be difficult to immediately obtain urine and blood, saliva and fingerprints could be effective alternative specimens for drug testing. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

SiC Nanowires Synthesized by Rapidly Heating a Mixture of SiO and Arc-Discharge Plasma Pretreated Carbon Black

PubMed Central

2009-01-01

SiC nanowires have been synthesized at 1,600 °C by using a simple and low-cost method in a high-frequency induction furnace. The commercial SiO powder and the arc-discharge plasma pretreated carbon black were mixed and used as the source materials. The heating-up and reaction time is less than half an hour. It was found that most of the nanowires have core-shell SiC/SiO2nanostructures. The nucleation, precipitation, and growth processes were discussed in terms of the oxide-assisted cluster-solid mechanism. PMID:20596456

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

A nanocluster-based fluorescent sensor for sensitive hemoglobin detection.

PubMed

Yang, Dongqin; Meng, Huijie; Tu, Yifeng; Yan, Jilin

2017-08-01

In this report, a fluorescence sensor for sensitive detection of hemoglobin was developed. Gold nanoclusters were first synthesized with bovine serum albumin. It was found that both hydrogen peroxide and hemoglobin could weakly quench the fluorescence from the gold nanoclusters, but when these two were applied onto the nanolcusters simultaneously, a much improved quenching was resulted. This enhancing effect was proved to come from the catalytic generation of hydroxyl radical by hemoglobin. Under an optimized condition, the quenching linearly related to the concentration of hemoglobin in the range of 1-250nM, and a limit of detection as low as 0.36nM could be obtained. This provided a sensitive means for the quantification of Hb. The sensor was then successfully applied for blood analyses with simple sample pretreatment. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of Trace Available Heavy Metals in Soil Using Laser-Induced Breakdown Spectroscopy Assisted with Phase Transformation Method.

PubMed

Yi, Rongxing; Yang, Xinyan; Zhou, Ran; Li, Jiaming; Yu, Huiwu; Hao, Zhongqi; Guo, Lianbo; Li, Xiangyou; Lu, Yongfeng; Zeng, Xiaoyan

2018-05-18

To detect available heavy metals in soil using laser-induced breakdown spectroscopy (LIBS) and improve its poor detection sensitivity, a simple and low cost sample pretreatment method named solid-liquid-solid transformation was proposed. By this method, available heavy metals were extracted from soil through ultrasonic vibration and centrifuging and then deposited on a glass slide. Utilization of this solid-liquid-solid transformation method, available Cd and Pb elements in soil were detected successfully. The results show that the regression coefficients of calibration curves for soil analyses reach to more than 0.98. The limits of detection could reach to 0.067 and 0.94 ppm for available Cd and Pb elements in soil under optimized conditions, respectively, which are much better than those obtained by conventional LIBS.

Condensation nucleation light scattering detection with ion chromatography for direct determination of glyphosate and its metabolite in water.

PubMed

You, Jing; Koropchak, John A

2003-03-14

An ion chromatography-condensation nucleation light scattering detection (IC-CNLSD) method was successfully used to directly analyze glyphosate, a polar pesticide, and aminomethylphosaphonic acid, the major metabolite of glyphosate, in water without need of pre-treatment or derivatization. CNLSD gave a LOD of 53 ng/ml for glyphosate, which is much lower than the maximum contaminant level of 700 ng/ml for drinking water issued by the US Environmental Protection Agency. Spiked analytes in different matrixes were tested. A diluted commercial herbicide containing glyphosate was also evaluated. Compared to other reported methods, the IC-CNLSD method has no need of sample derivatization, pre-concentration, and mobile phase conductivity suppression. It is simple, fast and inexpensive. IC-CNLSD is an ideal direct detection technique for such pesticides without chromophores or fluorophores.

Fast transient analysis and first-stage collision-induced dissociation with the flowing atmospheric-pressure afterglow ionization source to improve analyte detection and identification.

PubMed

Shelley, Jacob T; Hieftje, Gary M

2010-04-01

The recent development of ambient desorption/ionization mass spectrometry (ADI-MS) has enabled fast, simple analysis of many different sample types. The ADI-MS sources have numerous advantages, including little or no required sample pre-treatment, simple mass spectra, and direct analysis of solids and liquids. However, problems of competitive ionization and limited fragmentation require sample-constituent separation, high mass accuracy, and/or tandem mass spectrometry (MS/MS) to detect, identify, and quantify unknown analytes. To maintain the inherent high throughput of ADI-MS, it is essential for the ion source/mass analyzer combination to measure fast transient signals and provide structural information. In the current study, the flowing atmospheric-pressure afterglow (FAPA) ionization source is coupled with a time-of-flight mass spectrometer (TOF-MS) to analyze fast transient signals (<500 ms FWHM). It was found that gas chromatography (GC) coupled with the FAPA source resulted in a reproducible (<5% RSD) and sensitive (detection limits of <6 fmol for a mixture of herbicides) system with analysis times of ca. 5 min. Introducing analytes to the FAPA in a transient was also shown to significantly reduce matrix effects caused by competitive ionization by minimizing the number and amount of constituents introduced into the ionization source. Additionally, MS/MS with FAPA-TOF-MS, enabling analyte identification, was performed via first-stage collision-induced dissociation (CID). Lastly, molecular and structural information was obtained across a fast transient peak by modulating the conditions that caused the first-stage CID.

Estimation of nitrite in source-separated nitrified urine with UV spectrophotometry.

PubMed

Mašić, Alma; Santos, Ana T L; Etter, Bastian; Udert, Kai M; Villez, Kris

2015-11-15

Monitoring of nitrite is essential for an immediate response and prevention of irreversible failure of decentralized biological urine nitrification reactors. Although a few sensors are available for nitrite measurement, none of them are suitable for applications in which both nitrite and nitrate are present in very high concentrations. Such is the case in collected source-separated urine, stabilized by nitrification for long-term storage. Ultraviolet (UV) spectrophotometry in combination with chemometrics is a promising option for monitoring of nitrite. In this study, an immersible in situ UV sensor is investigated for the first time so to establish a relationship between UV absorbance spectra and nitrite concentrations in nitrified urine. The study focuses on the effects of suspended particles and saturation on the absorbance spectra and the chemometric model performance. Detailed analysis indicates that suspended particles in nitrified urine have a negligible effect on nitrite estimation, concluding that sample filtration is not necessary as pretreatment. In contrast, saturation due to very high concentrations affects the model performance severely, suggesting dilution as an essential sample preparation step. However, this can also be mitigated by simple removal of the saturated, lower end of the UV absorbance spectra, and extraction of information from the secondary, weaker nitrite absorbance peak. This approach allows for estimation of nitrite with a simple chemometric model and without sample dilution. These results are promising for a practical application of the UV sensor as an in situ nitrite measurement in a urine nitrification reactor given the exceptional quality of the nitrite estimates in comparison to previous studies. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

Detection of adenosine triphosphate through polymerization-induced aggregation of actin-conjugated gold/silver nanorods.

PubMed

Liao, Yu-Ju; Shiang, Yen-Chun; Chen, Li-Yi; Hsu, Chia-Lun; Huang, Chih-Ching; Chang, Huan-Tsung

2013-11-08

We have developed a simple and selective nanosensor for the optical detection of adenosine triphosphate (ATP) using globular actin-conjugated gold/silver nanorods (G-actin-Au/Ag NRs). By simply mixing G-actin and Au/Ag NRs (length ~56 nm and diameter ~12 nm), G-actin-Au/Ag NRs were prepared which were stable in physiological solutions (25 mM Tris-HCl, 150 mM NaCl, 5.0 mM KCl, 3.0 mM MgCl2 and 1.0 mM CaCl2; pH 7.4). Introduction of ATP into the G-actin-Au/Ag NR solutions in the presence of excess G-actin induced the formation of filamentous actin-conjugated Au/Ag NR aggregates through ATP-induced polymerization of G-actin. When compared to G-actin-modified spherical Au nanoparticles having a size of 13 nm or 56 nm, G-actin-Au/Ag NRs provided better sensitivity for ATP, mainly because the longitudinal surface plasmon absorbance of the Au/Ag NR has a more sensitive response to aggregation. This G-actin-Au/Ag NR probe provided high sensitivity (limit of detection 25 nM) for ATP with remarkable selectivity (>10-fold) over other adenine nucleotides (adenosine, adenosine monophosphate and adenosine diphosphate) and nucleoside triphosphates (guanosine triphosphate, cytidine triphosphate and uridine triphosphate). It also allowed the determination of ATP concentrations in plasma samples without conducting tedious sample pretreatments; the only necessary step was simple dilution. Our experimental results are in good agreement with those obtained from a commercial luciferin-luciferase bioluminescence assay. Our simple, sensitive and selective approach appears to have a practical potential for the clinical diagnosis of diseases (e.g. cystic fibrosis) associated with changes in ATP concentrations.

Detection of adenosine triphosphate through polymerization-induced aggregation of actin-conjugated gold/silver nanorods

NASA Astrophysics Data System (ADS)

Liao, Yu-Ju; Shiang, Yen-Chun; Chen, Li-Yi; Hsu, Chia-Lun; Huang, Chih-Ching; Chang, Huan-Tsung

2013-11-01

We have developed a simple and selective nanosensor for the optical detection of adenosine triphosphate (ATP) using globular actin-conjugated gold/silver nanorods (G-actin-Au/Ag NRs). By simply mixing G-actin and Au/Ag NRs (length ˜56 nm and diameter ˜12 nm), G-actin-Au/Ag NRs were prepared which were stable in physiological solutions (25 mM Tris-HCl, 150 mM NaCl, 5.0 mM KCl, 3.0 mM MgCl2 and 1.0 mM CaCl2; pH 7.4). Introduction of ATP into the G-actin-Au/Ag NR solutions in the presence of excess G-actin induced the formation of filamentous actin-conjugated Au/Ag NR aggregates through ATP-induced polymerization of G-actin. When compared to G-actin-modified spherical Au nanoparticles having a size of 13 nm or 56 nm, G-actin-Au/Ag NRs provided better sensitivity for ATP, mainly because the longitudinal surface plasmon absorbance of the Au/Ag NR has a more sensitive response to aggregation. This G-actin-Au/Ag NR probe provided high sensitivity (limit of detection 25 nM) for ATP with remarkable selectivity (>10-fold) over other adenine nucleotides (adenosine, adenosine monophosphate and adenosine diphosphate) and nucleoside triphosphates (guanosine triphosphate, cytidine triphosphate and uridine triphosphate). It also allowed the determination of ATP concentrations in plasma samples without conducting tedious sample pretreatments; the only necessary step was simple dilution. Our experimental results are in good agreement with those obtained from a commercial luciferin-luciferase bioluminescence assay. Our simple, sensitive and selective approach appears to have a practical potential for the clinical diagnosis of diseases (e.g. cystic fibrosis) associated with changes in ATP concentrations.

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.

A simple and efficient HPLC method for benznidazole dosage in human breast milk.

PubMed

Marson, María E; Padró, Juan M; Reta, Mario R; Altcheh, Jaime; García-Bournissen, Facundo; Mastrantonio, Guido

2013-08-01

Due to migration, Chagas disease is a significant public health problem in Latin America, and in other nonendemic regions. The 2 drugs currently available for the treatment, nifurtimox and benznidazole (BNZ), are associated with a high risk of toxicity in therapeutic doses. Excretion of drug into human breast milk is a potential source of unwanted exposure and pharmacologic effects in the nursing infant. However, this phenomenon was not evaluated until now, and measurement techniques for both drugs in milk were not developed. In this work, we described the development of a simple and fast method to quantify BNZ in human milk using a pretreatment that involves acid protein precipitation followed by tandem microfiltration, and reverse phase high-performance liquid chromatography/ultraviolet analysis. It is simple because it takes only 3 steps to obtain a clean extracted solution that is ready to inject into the high-performance liquid chromatography equipment. It is fast because a complete analysis of a sample takes only 36 minutes. Although the human breast milk composition is very variable, and lipids are one of the most difficult compounds to clean up on a milk sample, the procedure has proven to be robust and sensitive with a limit of detection of 0.3 μg/mL and quantization of 0.9 μg/mL. Despite a 70% recovery value, which could be considered a relatively low result, this recovery is reproducible (coefficient of variation <10%) and the analytical response under the linear range is very good (r = 0.9969 adjusted). Real samples of human breast milk from patients in treatment with BNZ were dosed to support the validation process of the method. The method described is fast, specific, accurate, precise, and sufficiently sensitive in the clinical context for the quantification of BNZ in human milk. For all these reasons, it is suitable for clinical risk evaluation studies.

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®.

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

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.

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.

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.

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 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.

[Development of sample pretreatment techniques-rapid detection coupling methods for food security analysis].

PubMed

Huang, Yichun; Ding, Weiwei; Zhang, Zhuomin; Li, Gongke

2013-07-01

This paper summarizes the recent developments of the rapid detection methods for food security, such as sensors, optical techniques, portable spectral analysis, enzyme-linked immunosorbent assay, portable gas chromatograph, etc. Additionally, the applications of these rapid detection methods coupled with sample pretreatment techniques in real food security analysis are reviewed. The coupling technique has the potential to provide references to establish the selective, precise and quantitative rapid detection methods in food security analysis.

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.

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.

A simple and sensitive enzymatic method for cholesterol quantification in macrophages and foam cells

PubMed Central

Robinet, Peggy; Wang, Zeneng; Hazen, Stanley L.; Smith, Jonathan D.

2010-01-01

A precise and sensitive method for measuring cellular free and esterified cholesterol is required in order to perform studies of macrophage cholesterol loading, metabolism, storage, and efflux. Until now, the use of an enzymatic cholesterol assay, commonly used for aqueous phase plasma cholesterol assays, has not been optimized for use with solid phase samples such as cells, due to inefficient solubilization of total cholesterol in enzyme compatible solvents. We present an efficient solubilization protocol compatible with an enzymatic cholesterol assay that does not require chemical saponification or chromatographic separation. Another issue with enzyme compatible solvents is the presence of endogenous peroxides that interfere with the enzymatic cholesterol assay. We overcame this obstacle by pretreatment of the reaction solution with the enzyme catalase, which consumed endogenous peroxides resulting in reduced background and increased sensitivity in our method. Finally, we demonstrated that this method for cholesterol quantification in macrophages yields results that are comparable to those measured by stable isotope dilution gas chromatography with mass spectrometry detection. In conclusion, we describe a sensitive, simple, and high-throughput enzymatic method to quantify cholesterol in complex matrices such as cells. PMID:20688754

A Contactless Capacitance Detection System for Microchip Capillary Electrophoresis

NASA Astrophysics Data System (ADS)

Wu, Peter

2008-05-01

The design, construction and operation of a simple, inexpensive and compact high voltage power supply for use in conjunction with a simple cross, capillary electrophoresis microchip is presented. The detection system utilizes a single high voltage power supply (15 kV), a voltage divider network for obtaining the required voltages for enabling a gated injection valve, and two high voltage relays for switching between the open and closed gate sequences of the injection. The system is used to determine sodium monofluoroacetate (MFA) concentration in diluted fruit juices and tap water. A separation buffer consisting of 20 mM citric acid and histidine at pH 3.5 enabled the detection of the anion in diluted apple juice, cranberry juice, and orange juice without lengthy sample pretreatments. Limit of detection in diluted juices and tap water were determined to be 125, 167, 138, and 173 mg/L for tap water, apple juice, cranberry juice, and orange juice, respectively, based upon an S/N of 3:1. The total analysis time for detecting the MFA anion in fruit juices was less than 5 min, which represents a considerable reduction in analysis time compared to other analytical methods currently used in food analysis.

Derivatization Ion Chromatography for the Determination of Monoethanolamine in Presence of Hydrazine in PHWR Steam-Water Circuits

PubMed Central

D., Ayushi; Sengupta, Arijit; Kumar, Sangita D.; Kumbhar, A. G.; Venkateswaran, G.

2011-01-01

A simple, rapid and accurate method for the determination of monoethanolamine (MEA) in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4 mM tartaric acid, 20% acetone and 0.05 mM HNO3 was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+ and NH4  + were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1 μg mL−1 and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples. PMID:21785596

Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

PubMed

Xu, Jiao-Jiao; Zhou, Jian; Huang, Bai-Fen; Cai, Zeng-Xuan; Xu, Xiao-Min; Ren, Yi-Ping

2016-06-01

A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Combination of nano-material enrichment and dead-end filtration for uniform and rapid sample preparation in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Wu, Zengnan; Khan, Mashooq; Mao, Sifeng; Lin, Ling; Lin, Jin-Ming

2018-05-01

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a fast analysis tool for the detection of a wide range of analytes. However, heterogeneous distribution of matrix/analyte cocrystal, variation in signal intensity and poor experimental reproducibility at different locations of the same spot means difficulty in quantitative analysis. In this work, carbon nanotubes (CNTs) were employed as adsorbent for analyte cum matrix on a conductive porous membrane as a novel mass target plate. The sample pretreatment step was achieved by enrichment and dead-end filtration and dried by a solid-liquid separation. This approach enables the homogeneous distribution of analyte in the matrix, good shot-to-shot reproducibility in signals and quantitative detection of peptide and protein at different concentrations with correlation coefficient (R 2 ) of 0.9920 and 0.9909, respectively. The simple preparation of sample in a short time, uniform distribution of analyte, easy quantitative detection, and high reproducibility makes this technique useful and may diversify the application of MALDI-MS for quantitative detection of a variety of proteins. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

PubMed

Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

2010-07-01

A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

Pulsating potentiometric titration technique for assay of dissolved oxygen in water at trace level.

PubMed

Sahoo, P; Ananthanarayanan, R; Malathi, N; Rajiniganth, M P; Murali, N; Swaminathan, P

2010-06-11

A simple but high performance potentiometric titration technique using pulsating sensors has been developed for assay of dissolved oxygen (DO) in water samples down to 10.0 microg L(-1) levels. The technique involves Winkler titration chemistry, commonly used for determination of dissolved oxygen in water at mg L(-1) levels, with modification in methodology for accurate detection of end point even at 10.0 microg L(-1) levels DO present in the sample. An indigenously built sampling cum pretreatment vessel has been deployed for collection and chemical fixing of dissolved oxygen in water samples from flowing water line without exposure to air. A potentiometric titration facility using pulsating sensors developed in-house is used to carry out titration. The power of the titration technique has been realised in estimation of very dilute solution of iodine equivalent to 10 microg L(-1) O(2). Finally, several water samples containing dissolved oxygen from mg L(-1) to microg L(-1) levels were successfully analysed with excellent reproducibility using this new technique. The precision in measurement of DO in water at 10 microg L(-1) O(2) level is 0.14 (n=5), RSD: 1.4%. Probably for the first time a potentiometric titration technique has been successfully deployed for assay of dissolved oxygen in water samples at 10 microg L(-1) levels. Copyright 2010 Elsevier B.V. All rights reserved.

Surfactant sodium lauryl sulfate enhances skin vaccination: molecular characterization via a novel technique using ultrafiltration capillaries and mass spectrometric proteomics.

PubMed

Huang, Chun-Ming; Wang, Chao-Cheng; Kawai, Mikako; Barnes, Stephen; Elmets, Craig A

2006-03-01

The skin is a highly accessible organ and thus provides an attractive immune environment for cost-effective, simple, and needle-free delivery of vaccines and immunomodulators. In this study, we pretreated mouse skin with an anionic surfactant, sodium lauryl sulfate (SLS), for a short period of time (10 min) followed by epicutaneous vaccination with hen egg lysozyme antigen. We demonstrated for the first time that pretreatment of skin with surfactant SLS significantly enhances the production of antibody to hen egg lysozyme. Short term pretreatment with SLS disorganized the stratum corneum, extracted partial lamellar lipids, induced the maturation of Langerhans cells, and did not result in epidermis thickening. To reveal the mechanism underlying these changes, particularly at the molecular level, we used a novel proteomic technique using ultrafiltration capillaries and mass spectrometry to identify in vivo proteins/peptides secreted in the SLS-pretreated skin. Two secretory proteins, named as calcium-binding protein S100A9 and thymosin beta4, were identified by this novel technique. These two proteins thus may provide new insight into the enhancing effect of surfactants on skin vaccination.

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...

A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

PubMed

Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

2018-06-15

Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Simultaneous determination of six synthetic phenolic antioxidants in edible oils using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography with diode array detection.

PubMed

Xu, Shuangjiao; Liu, Liangliang; Wang, Yanqin; Zhou, Dayun; Kuang, Meng; Fang, Dan; Yang, Weihua; Wei, Shoujun; Xiao, Aiping; Ma, Lei

2016-08-01

A simple, rapid, organic-solvent- and sample-saving pretreatment technique, called dispersive liquid-liquid microextraction, was developed for the determination of six synthetic phenolic antioxidants from edible oils before high-performance liquid chromatography with diode array detection. The entire procedure was composed of a two-step microextraction and a centrifugal process and could be finished in about 5 min, only consuming only 25 mg of sample and 1 mL of the organic solvent for each extraction. The influences of several important parameters on the microextraction efficiency were thoroughly investigated. Recovery assays for oil samples were spiked at three concentration levels, 50, 100 and 200 mg/kg, and provided recoveries in the 86.3-102.5% range with a relative standard deviation below 3.5%. The intra-day and inter-day precisions for the analysis were less than 3.8%. The proposed method was successfully applied for the determination of synthetic phenolic antioxidants in different oil samples, and satisfactory results were obtained. Thus, the developed method represents a viable alternative for the quality control of synthetic phenolic antioxidant concentrations in edible oils. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bulk Cutting of Carbon Nanotubes Using Electron Beam Irradiation

NASA Technical Reports Server (NTRS)

Schmidt, Howard K. (Inventor); Hauge, Robert H. (Inventor); Smalley, Richard E. (Inventor); Rauwald, Urs (Inventor); Kittrell, W. Carter (Inventor); Ziegler, Kirk J. (Inventor); Gu, Zhenning (Inventor)

2013-01-01

According to some embodiments, the present invention provides a method for attaining short carbon nanotubes utilizing electron beam irradiation, for example, of a carbon nanotube sample. The sample may be pretreated, for example by oxonation. The pretreatment may introduce defects to the sidewalls of the nanotubes. The method is shown to produces nanotubes with a distribution of lengths, with the majority of lengths shorter than 100 tun. Further, the median length of the nanotubes is between about 20 nm and about 100 nm.

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.

The conversion of lignocellulosics to fermentable sugars - A survey of current research and applications to CELSS

NASA Technical Reports Server (NTRS)

Petersen, Gene R.; Baresi, Larry

1990-01-01

This report provides an overview options for converting lignocellulosics into fermentable sugars in CELSS. A requirement for pretreatment is shown. Physical-chemical and enzymatic hydrolysis processes for producing fermentable sugars are discussed. At present physical-chemical methods are the simplest and best characterized options, but enzymatic processes will be the likely method of choice in the future. The use of pentose sugars by microorganisms to produce edibles is possible. The use of mycelial food production on pretreated but not hydrolyzed lignocellulosics is also possible. Simple trade-off analyses to regenerate waste lignocellulosics for two pathways are made, one of which is compared to complete oxidation.

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.

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...

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

Demonstration and Optimization of BNFL's Pulsed Jet Mixing and RFD Sampling Systems Using NCAW Simulant

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

JR Bontha; GR Golcar; N Hannigan

2000-08-29

The BNFL Inc. flowsheet for the pretreatment and vitrification of the Hanford High Level Tank waste includes the use of several hundred Reverse Flow Diverters (RFDs) for sampling and transferring the radioactive slurries and Pulsed Jet mixers to homogenize or suspend the tank contents. The Pulsed Jet mixing and the RFD sampling devices represent very simple and efficient methods to mix and sample slurries, respectively, using compressed air to achieve the desired operation. The equipment has no moving parts, which makes them very suitable for mixing and sampling highly radioactive wastes. However, the effectiveness of the mixing and sampling systemsmore » are yet to be demonstrated when dealing with Hanford slurries, which exhibit a wide range of physical and theological properties. This report describes the results of the testing of BNFL's Pulsed Jet mixing and RFD sampling systems in a 13-ft ID and 15-ft height dish-bottomed tank at Battelle's 336 building high-bay facility using AZ-101/102 simulants containing up to 36-wt% insoluble solids. The specific objectives of the work were to: Demonstrate the effectiveness of the Pulsed Jet mixing system to thoroughly homogenize Hanford-type slurries over a range of solids loading; Minimize/optimize air usage by changing sequencing of the Pulsed Jet mixers or by altering cycle times; and Demonstrate that the RFD sampler can obtain representative samples of the slurry up to the maximum RPP-WTP baseline concentration of 25-wt%.« less

Organic acid pretreatment of oil palm trunk: effect on enzymatic saccharification and ethanol production.

PubMed

Rattanaporn, Kittipong; Tantayotai, Prapakorn; Phusantisampan, Theerawut; Pornwongthong, Peerapong; Sriariyanun, Malinee

2018-04-01

Effective lignocellulosic biomass saccharification is one of the crucial requirements of biofuel production via fermentation process. Organic acid pretreatments have been gained much interests as one of the high potential methods for promoting enzymatic saccharification of lignocellulosic materials due to their lower hazardous properties and lower production of inhibitory by-products of fermentation than typical chemical pretreatment methods. In this study, three organic acids, including acetic acid, oxalic acid, and citric acid, were examined for improvement of enzymatic saccharification and bioethanol production from oil palm trunk biomass. Based on response surface methodology, oxalic acid pretreated biomass released the maximum reducing sugar of 144 mg/g-pretreated biomass at the optimum condition, which was higher than untreated samples for 2.30 times. The released sugar yield of oil palm trunk also corresponded to the results of FT-IR analysis, which revealed the physical modification of cellulose and hemicellulose surface structures of pretreated biomass. Nevertheless, citric acid pretreatment is the most efficient pretreatment method to improve bioethanol fermentation of Saccharomyces cerevisiae TISTR 5606 at 1.94 times higher than untreated biomass. These results highlighted the selection of organic acid pretreatment as a potential method for biofuel production from oil palm trunk feedstocks.

On-chip sample pretreatment using a porous polymer monolithic column for solid-phase microextraction and chemiluminescence determination of catechins in green tea.

PubMed

Lin, Ling; Chen, Hui; Wei, Huibin; Wang, Feng; Lin, Jin-Ming

2011-10-21

A porous polymer monolithic column for solid-phase microextraction and chemiluminescence detection was integrated into a simple microfluidic chip for the extraction and determination of catechins in green tea. The porous polymer was prepared by poly(glycidyl methacrylate-co-ethylene dimethacrylate) and modified with ethylenediamine. Catechins can be concentrated in the porous polymer monolithic column and react with potassium permanganate to give chemiluminescence. The microfluidic chip is reusable with high sensitivity and very low reagent consumption. The on-line preconcentration and detection can be realized without an elution step. The enrichment factor was calculated to be about 20 for catechins. The relative chemiluminescence intensity increased linearly with concentration of catechin from 5.0 × 10(-9) to 1.0 × 10(-6) M and the limit of detection was 1.0 × 10(-9) M. The proposed method was applied to determine catechin in green tea. The recoveries are from 90% to 110% which benefits the actual application for green tea samples.

Liquid chromatographic determination of urinary 5-methyl-2'-deoxycytidine and pseudouridine as potential biological markers for leukaemia.

PubMed

Zambonin, C G; Aresta, A; Palmisano, F; Specchia, G; Liso, V

1999-12-01

A simple reversed-phase liquid chromatographic (LC) method for the determination of urinary 5-methyl-2'-deoxycytidine (m5dCyd), recently claimed (on the basis of an imuno-technique) to be a potential marker for leukaemia, has been developed. Sample pre-treatment is based on a microcolumn clean-up step with an average recovery of 79% and a RSD of 3%. Detection limit was 0.2 microg/ml which is about tenfold lower than levels previously measured by an ELISA method in urine of healthy individuals. The creatinine (Cre) excretion, necessary for normalising the m5dCyd excretion, was evaluated by ion-pair liquid chromatography which permitted the simultaneous determination of pseudouridine (psi), a modified nucleoside also potentially useful as a marker for leukaemia. The described LC procedures were applied to the analysis of urine samples from healthy individuals and leukaemia patients. While the urinary psi/Cre ratio was found significantly increased for leukaemia patients, the urinary m5dCyd levels in healthy individuals were below the detection limits and did not increase in presence of the malignant disease.

Direct immersion single drop micro-extraction method for multi-class pesticides analysis in mango using GC-MS.

PubMed

Pano-Farias, Norma S; Ceballos-Magaña, Silvia G; Muñiz-Valencia, Roberto; Jurado, Jose M; Alcázar, Ángela; Aguayo-Villarreal, Ismael A

2017-12-15

Due the negative effects of pesticides on environment and human health, more efficient and environmentally friendly methods are needed. In this sense, a simple, fast, free from memory effects and economical direct-immersion single drop micro-extraction (SDME) method and GC-MS for multi-class pesticides determination in mango samples was developed. Sample pre-treatment using ultrasound-assisted solvent extraction and factors affecting the SDME procedure (extractant solvent, drop volume, stirring rate, ionic strength, time, pH and temperature) were optimized using factorial experimental design. This method presented high sensitive (LOD: 0.14-169.20μgkg -1 ), acceptable precision (RSD: 0.7-19.1%), satisfactory recovery (69-119%) and high enrichment factors (20-722). Several obtained LOQs are below the MRLs established by the European Commission; therefore, the method could be applied for pesticides determination in routing analysis and custom laboratories. Moreover, this method has shown to be suitable for determination of some of the studied pesticides in lime, melon, papaya, banana, tomato, and lettuce. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fast Determination of Yttrium and Rare Earth Elements in Seawater by Inductively Coupled Plasma-Mass Spectrometry after Online Flow Injection Pretreatment.

PubMed

Zhu, Zuhao; Zheng, Airong

2018-02-23

A method for daily monitoring of yttrium and rare earth elements (YREEs) in seawater using a cheap flow injection system online coupled to inductively coupled plasma-mass spectrometry is reported. Toyopearl AF Chelate 650M ® resin permits separation and concentration of YREEs using a simple external calibration. A running cycle consumed 6 mL sample and took 5.3 min, providing a throughput of 11 samples per hour. Linear ranges were up to 200 ng kg -1 except Tm (100 ng kg -1 ). The precision of the method was <6% (RSDs, n = 5), and recoveries ranged from 93% to 106%. Limits of detection (LODs) were in the range 0.002 ng kg -1 (Tm) to 0.078 ng kg -1 (Ce). Good agreement between YREEs concentrations in CASS-4 and SLEW-3 obtained in this work and results from other studies was observed. The proposed method was applied to the determination of YREEs in seawater from the Jiulong River Estuary and the Taiwan Strait.

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.

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.

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.

Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

PubMed

Zhang, Gai

2012-01-01

Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil. © 2011 Institute of Food Technologists®

Using detergent to enhance detection sensitivity of African trypanosomes in human CSF and blood by loop-mediated isothermal amplification (LAMP).

PubMed

Grab, Dennis J; Nikolskaia, Olga V; Inoue, Noboru; Thekisoe, Oriel M M; Morrison, Liam J; Gibson, Wendy; Dumler, J Stephen

2011-08-01

The loop-mediated isothermal amplification (LAMP) assay, with its advantages of simplicity, rapidity and cost effectiveness, has evolved as one of the most sensitive and specific methods for the detection of a broad range of pathogenic microorganisms including African trypanosomes. While many LAMP-based assays are sufficiently sensitive to detect DNA well below the amount present in a single parasite, the detection limit of the assay is restricted by the number of parasites present in the volume of sample assayed; i.e. 1 per µL or 10(3) per mL. We hypothesized that clinical sensitivities that mimic analytical limits based on parasite DNA could be approached or even obtained by simply adding detergent to the samples prior to LAMP assay. For proof of principle we used two different LAMP assays capable of detecting 0.1 fg genomic DNA (0.001 parasite). The assay was tested on dilution series of intact bloodstream form Trypanosoma brucei rhodesiense in human cerebrospinal fluid (CSF) or blood with or without the addition of the detergent Triton X-100 and 60 min incubation at ambient temperature. With human CSF and in the absence of detergent, the LAMP detection limit for live intact parasites using 1 µL of CSF as the source of template was at best 10(3) parasites/mL. Remarkably, detergent enhanced LAMP assay reaches sensitivity about 100 to 1000-fold lower; i.e. 10 to 1 parasite/mL. Similar detergent-mediated increases in LAMP assay analytical sensitivity were also found using DNA extracted from filter paper cards containing blood pretreated with detergent before card spotting or blood samples spotted on detergent pretreated cards. This simple procedure for the enhanced detection of live African trypanosomes in biological fluids by LAMP paves the way for the adaptation of LAMP for the economical and sensitive diagnosis of other protozoan parasites and microorganisms that cause diseases that plague the developing world.

Development of an ionic-liquid-based dispersive liquid-liquid microextraction method for the determination of antichagasic drugs in human breast milk: Optimization by central composite design.

PubMed

Padró, Juan M; Pellegrino Vidal, Rocío B; Echevarria, Romina N; Califano, Alicia N; Reta, Mario R

2015-05-01

Chagas disease constitutes a major public health problem in Latin America. Human breast milk is a biological sample of great importance for the analysis of therapeutic drugs, as unwanted exposure through breast milk could result in pharmacological effects in the nursing infant. Thus, the goal of breast milk drug analysis is to inquire to which extent a neonate may be exposed to a drug during lactation. In this work, we developed an analytical technique to quantify benznidazole and nifurtimox (the two antichagasic drugs currently available for medical treatment) in human breast milk, with a simple sample pretreatment followed by an ionic-liquid-based dispersive liquid-liquid microextraction combined with high-performance liquid chromatography and UV detection. For this technique, the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate has been used as the "extraction solvent." A central composite design was used to find the optimum values for the significant variables affecting the extraction process: volume of ionic liquid, volume of dispersant solvent, ionic strength, and pH. At the optimum working conditions, the average recoveries were 77.5 and 89.7%, the limits of detection were 0.06 and 0.09 μg/mL and the interday reproducibilities were 6.25 and 5.77% for benznidazole and nifurtimox, respectively. The proposed methodology can be considered sensitive, simple, robust, accurate, and green. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Microemulsion-based lycopene extraction: Effect of surfactants, co-surfactants and pretreatments.

PubMed

Amiri-Rigi, Atefeh; Abbasi, Soleiman

2016-04-15

Lycopene is a potent antioxidant that has received extensive attention recently. Due to the challenges encountered with current methods of lycopene extraction using hazardous solvents, industry calls for a greener, safer and more efficient process. The main purpose of present study was application of microemulsion technique to extract lycopene from tomato pomace. In this respect, the effect of eight different surfactants, four different co-surfactants, and ultrasound and enzyme pretreatments on lycopene extraction efficiency was examined. Experimental results revealed that application of combined ultrasound and enzyme pretreatments, saponin as a natural surfactant, and glycerol as a co-surfactant, in the bicontinuous region of microemulsion was the optimal experimental conditions resulting in a microemulsion containing 409.68±0.68 μg/glycopene. The high lycopene concentration achieved, indicates that microemulsion technique, using a low-cost natural surfactant could be promising for a simple and safe separation of lycopene from tomato pomace and possibly from tomato industrial wastes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Liquid nitrogen pretreatment of eucalyptus sawdust and rice hull for enhanced enzymatic saccharification.

PubMed

Castoldi, Rafael; Correa, Vanesa G; de Morais, Gutierrez Rodrigues; de Souza, Cristina G M; Bracht, Adelar; Peralta, Rosely A; Peralta-Muniz Moreira, Regina F; Peralta, Rosane M

2017-01-01

In this work, liquid nitrogen was used for the first time in the pretreatment of plant biomasses for purposes of enzymatic saccharification. After treatment (cryocrushing), the initial rates of the enzymatic hydrolysis of eucalyptus sawdust and rice hull were increased more than ten-fold. Cryocrushing did not modify significantly the contents of cellulose, hemicellulose and lignin in both eucalyptus sawdust and rice hulls. However, substantial disorganization of the lignocellulosic materials in consequence of the pretreatment could be observed by electron microscopy. Cryocrushing was highly efficient in improving the saccharification of the holocellulose component of the plant biomasses (from 4.3% to 54.1% for eucalyptus sawdust and from 3.9% to 40.6% for rice hull). It is important to emphasize that it consists in a simple operation with low requirements of water and chemicals, no corrosion, no release of products such as soluble phenolics, furfural and hydroxymethylfurfural and no waste generation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Understanding the mechanisms of lipid extraction from microalga Chlamydomonas reinhardtii after electrical field solicitations and mechanical stress within a microfluidic device.

PubMed

Bensalem, Sakina; Lopes, Filipa; Bodénès, Pierre; Pareau, Dominique; Français, Olivier; Le Pioufle, Bruno

2018-06-01

One way envisioned to overcome part of the issues biodiesel production encounters today is to develop a simple, economically viable and eco-friendly process for the extraction of lipids from microalgae. This study investigates the lipid extraction efficiency from the microalga Chlamydomonas reinhardtii as well as the underlying mechanisms. We propose a new methodology combining a pulsed electric field (PEF) application and mechanical stresses as a pretreatment to improve lipid extraction with solvents. Cells enriched in lipids are therefore submitted to electric field pulses creating pores on the cell membrane and then subjected to a mechanical stress by applying cyclic pressures on the cell wall (using a microfluidic device). Results showed an increase in lipid extraction when cells were pretreated by the combination of both methods. Microscopic observations showed that both pretreatments affect the cell structure. Finally, the dependency of solvent lipid extraction efficiency with the cell wall structure is discussed. Copyright © 2018 Elsevier Ltd. All rights reserved.

Lipid overloading during liver regeneration causes delayed hepatocyte DNA replication by increasing ER stress in mice with simple hepatic steatosis.

PubMed

Hamano, Mina; Ezaki, Hisao; Kiso, Shinichi; Furuta, Kunimaro; Egawa, Mayumi; Kizu, Takashi; Chatani, Norihiro; Kamada, Yoshihiro; Yoshida, Yuichi; Takehara, Tetsuo

2014-02-01

Impaired fatty liver regeneration has already been reported in many genetic modification models. However, in diet-induced simple hepatic steatosis, which showed similar phenotype with clinical pathology, whether liver regeneration is impaired or not remains unclear. In this study, we evaluated liver regeneration in mice with diet-induced simple hepatic steatosis, and focused on excess lipid accumulation occurring during liver regeneration. Mice were fed high fat diet (HFD) or control diet for 9-10 weeks. We analyzed intrahepatic lipid accumulation, DNA replication, and various signaling pathways including cell proliferation and ER stress during liver regeneration after partial hepatectomy. In addition, some of mice were pretreated with tauroursodeoxycholic acid (TUDCA), a chemical chaperone which alleviates ER stress, and then we estimated TUDCA effects on liver regeneration. The peak of hepatocyte BrdU incorporation, the expression of proliferation cell nuclear antigen (PCNA) protein, and the expressions of cell cycle-related genes were observed in delayed time in HFD mice. The expression of phosphorylated Erk1/2 was also delayed in HFD mice. The amounts of liver triglyceride were at least twofold higher in HFD mice at each time point. Intrahepatic palmitic acid was increased especially in HFD mice. ER stress induced during liver regeneration was significantly higher in HFD mice. In HFD mice, pretreatment with TUDCA reduced ER stress and resulted in improvement of delayed liver regeneration. In simple hepatic steatosis, lipid overloading occurring during liver regeneration might be caused ER stress and results in delayed hepatocyte DNA replication.

Simultaneous determination of vancomycin and ceftazidime in cerebrospinal fluid in craniotomy patients by high-performance liquid chromatography.

PubMed

Ye, Guangming; Cai, Xuejian; Wang, Biao; Zhou, Zhongxian; Yu, Xiaohua; Wang, Weibin; Zhang, Jiandong; Wang, Yuhai; Dong, Jierong; Jiang, Yunyun

2008-11-04

A simple, accurate and rapid method for simultaneous analysis of vancomycin and ceftazidime in cerebrospinal fluid (CSF), utilizing high-performance liquid chromatography (HPLC), has been developed and thoroughly validated to satisfy strict FDA guidelines for bioanalytical methods. Protein precipitation was used as the sample pretreatment method. In order to increase the accuracy, tinidazole was chosen as the internal standard. Separation was achieved on a Diamonsil C18 column (200 mm x 4.6mm I.D., 5 microm) using a mobile phase composed of acetonitrile and acetate buffer (pH 3.5) (8:92, v/v) at room temperature (25 degrees C), and the detection wavelength was 240 nm. All the validation data, such as accuracy, precision, and inter-day repeatability, were within the required limits. The method was applied to determine vancomycin and ceftazidime concentrations in CSF in five craniotomy patients.

Application of I-structure though-glass interconnect filled with submicron gold particles to a hermetic sealing device

NASA Astrophysics Data System (ADS)

Nomura, Kazuya; Okada, Akiko; Shoji, Shuichi; Ogashiwa, Toshinori; Mizuno, Jun

2016-10-01

We propose hermetic sealing of a glass-to-glass structure with an I-structure through-glass interconnect via (TGV) filled with submicron Au particles. The top and bottom bumps and the TGV were formed by a simple filling process with a bump-patterned dry film resist. The sealing devices consisting of two glass substrates were bonded via Au interlayers. Vacuum ultraviolet irradiation in the presence of oxygen gas (VUV/O3) pretreatment was used for low-temperature Au-Au bonding at 200 °C. The bonded samples showed He leakage rates of less than 1.3  ×  10-9 Pa m3 s-1. The cross-sectional scanning electron microscope images of the fabricated I-structure TGV showed perfect adhesion between the I-structure TGV and glass substrate. These results indicate that the proposed I-structure TGV is suitable for hermetic sealing devices.

Detection of polychlorinated biphenyls in transformer oils in Vietnam by multiphoton ionization mass spectrometry using a far-ultraviolet femtosecond laser as an ionization source.

PubMed

Duong, Vu Thi Thuy; Duong, Vu; Lien, Nghiem Thi Ha; Imasaka, Tomoko; Tang, Yuanyuan; Shibuta, Shinpei; Hamachi, Akifumi; Hoa, Do Quang; Imasaka, Totaro

2016-03-01

Polychlorinated biphenyls (PCBs) in transformer and food oils were measured using gas chromatography combined with multiphoton ionization mass spectroscopy. An ultrashort laser pulse emitting in the far-ultraviolet region was utilized for efficient ionization of the analytes. Numerous signal peaks were clearly observed for a standard sample mixture of PCBs when the third and fourth harmonic emissions (267 and 200nm) of a femtosecond Ti:sapphire laser (800nm) were employed. The signal intensities were found to be greater when measured at 200nm compared with those measured at 267nm, providing lower detection limits especially for highly chlorinated PCBs at shorter wavelengths. After simple pretreatment using disposable columns, PCB congeners were measured and found to be present in the transformer oils used in Vietnam. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid determination of vitellogenin in fish plasma by anion exchange high performance liquid chromatography using postcolumn fluorescence derivatization with o-phthalaldehyde.

PubMed

Wu, Cuiqin; Yuan, Dongxing; Liu, Baomin

2006-12-01

An analytical method involving anion exchange high performance liquid chromatographic determination of vitellogenin (Vtg) in fish plasma after postcolumn fluorescence derivatization with o-phthalaldehyde (OPA) was developed. The retention time of Vtg was about 11 min. The reagent variables for derivatization were optimized. The fluorophore was excited at 335 nm and detected at 435 nm. A calibration curve was established ranging from 0.13 to 11.28 microg. The determination limit of Vtg was found to be as low as 0.13 microg. The spiked recovery was 93.6% and interassay variability was less than 4%. The method developed was used to determine Vtg in fish plasma obtained from red sea bream (Pagrosomus major), black porgy (Sparus macrocephalus) and skew band grunt (Hapalogenys nitens), without complicated sample pretreatment. The results confirmed that the method showed advantages of being simple, rapid, reproducible and sensitive.

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.

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.

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.

Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-01-01

A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

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.

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.

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.

Quantitative Proteomic Analysis of Optimal Cutting Temperature (OCT) Embedded Core-Needle Biopsy of Lung Cancer

NASA Astrophysics Data System (ADS)

Zhao, Xiaozheng; Huffman, Kenneth E.; Fujimoto, Junya; Canales, Jamie Rodriguez; Girard, Luc; Nie, Guangjun; Heymach, John V.; Wistuba, Igacio I.; Minna, John D.; Yu, Yonghao

2017-10-01

With recent advances in understanding the genomic underpinnings and oncogenic drivers of pathogenesis in different subtypes, it is increasingly clear that proper pretreatment diagnostics are essential for the choice of appropriate treatment options for non-small cell lung cancer (NSCLC). Tumor tissue preservation in optimal cutting temperature (OCT) compound is commonly used in the surgical suite. However, proteins recovered from OCT-embedded specimens pose a challenge for LC-MS/MS experiments, due to the large amounts of polymers present in OCT. Here we present a simple workflow for whole proteome analysis of OCT-embedded NSCLC tissue samples, which involves a simple trichloroacetic acid precipitation step. Comparisons of protein recovery between frozen versus OCT-embedded tissue showed excellent consistency with more than 9200 proteins identified. Using an isobaric labeling strategy, we quantified more than 5400 proteins in tumor versus normal OCT-embedded core needle biopsy samples. Gene ontology analysis indicated that a number of proliferative as well as squamous cell carcinoma (SqCC) marker proteins were overexpressed in the tumor, consistent with the patient's pathology based diagnosis of "poorly differentiated SqCC". Among the most downregulated proteins in the tumor sample, we noted a number of proteins with potential immunomodulatory functions. Finally, interrogation of the aberrantly expressed proteins using a candidate approach and cross-referencing with publicly available databases led to the identification of potential druggable targets in DNA replication and DNA damage repair pathways. We conclude that our approach allows LC-MS/MS proteomic analyses on OCT-embedded lung cancer specimens, opening the way to bring powerful proteomics into the clinic. [Figure not available: see fulltext.

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.

Causal Inference and the Comparative Interrupted Time Series Design: Findings from Within-Study Comparisons

ERIC Educational Resources Information Center

St. Clair, Travis; Hallberg, Kelly; Cook, Thomas D.

2014-01-01

Researchers are increasingly using comparative interrupted time series (CITS) designs to estimate the effects of programs and policies when randomized controlled trials are not feasible. In a simple interrupted time series design, researchers compare the pre-treatment values of a treatment group time series to post-treatment values in order to…

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

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.

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.

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.

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.

A simple pre-treatment of aluminium cookware to minimize aluminium transfer to food.

PubMed

Karbouj, Rim; Desloges, I; Nortier, P

2009-03-01

In this work, we studied aluminium leaching from cookware to food under the effect of citric acid that is commonly found in foods and beverages. The authors showed that boiling the cookware in water prior to cooking is suitable for the decrease of aluminium leaching into food by a factor up to sixty (with a corresponding decrease of the aluminium intake by consumers). The effect of the pre-treatment has been studied by scanning electron microscopy and X-Ray diffraction and the effect has been attributed to changes in the structure and morphology of the passivation layer, from an initial heterogeneous layer to a surface uniformly covered with fine needles of Boehmite (alpha-AlOOH).

[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.

Enrichment of Secondary Wastewater Sludge for Production of Hydrogen from Crude Glycerol and Comparative Evaluation of Mono-, Co- and Mixed-Culture Systems

PubMed Central

Pachapur, Vinayak Laxman; Kutty, Prianka; Brar, Satinder Kaur; Ramirez, Antonio Avalos

2016-01-01

Anaerobic digestion using mixed-culture with broader choice of pretreatments for hydrogen (H2) production was investigated. Pretreatment of wastewater sludge by five methods, such as heat, acid, base, microwave and chloroform was conducted using crude glycerol (CG) as substrate. Results for heat treatment (100 °C for 15 min) showed the highest H2 production across the pretreatment methods with 15.18 ± 0.26 mmol/L of medium at 30 °C in absence of complex media and nutrient solution. The heat-pretreated inoculum eliminated H2 consuming bacteria and produced twice as much as H2 as compared to other pretreatment methods. The fermentation conditions, such as CG concentration (1.23 to 24 g/L), percentage of inoculum size (InS) (1.23% to 24% v/v) along with initial pH (2.98 to 8.02) was tested using central composite design (CCD) with H2 production as response parameter. The maximum H2 production of 29.43 ± 0.71 mmol/L obtained at optimum conditions of 20 g/L CG, 20% InS and pH 7. Symbiotic correlation of pH over CG and InS had a significant (p-value: 0.0011) contribution to H2 production. The mixed-culture possessed better natural acclimatization activity for degrading CG, at substrate inhibition concentration and provided efficient inoculum conditions in comparison to mono- and co-culture systems. The heat pretreatment step used across mixed-culture system is simple, cheap and industrially applicable in comparison to mono-/co-culture systems for H2 production. PMID:26771607

A pretreatment method for grain size analysis of red mudstones

NASA Astrophysics Data System (ADS)

Jiang, Zaixing; Liu, Li'an

2011-11-01

Traditional sediment disaggregation methods work well for loose mud sediments, but not for tightly cemented mudstones by ferric oxide minerals. In this paper, a new pretreatment method for analyzing the grain size of red mudstones is presented. The experimental samples are Eocene red mudstones from the Dongying Depression, Bohai Bay Basin. The red mudstones are composed mainly of clay minerals, clastic sediments and ferric oxides that make the mudstones red and tightly compacted. The procedure of the method is as follows. Firstly, samples of the red mudstones were crushed into fragments with a diameter of 0.6-0.8 mm in size; secondly, the CBD (citrate-bicarbonate-dithionite) treatment was used to remove ferric oxides so that the cementation of intra-aggregates and inter-aggregates became weakened, and then 5% dilute hydrochloric acid was added to further remove the cements; thirdly, the fragments were further ground with a rubber pestle; lastly, an ultrasonicator was used to disaggregate the samples. After the treatment, the samples could then be used for grain size analysis or for other geological analyses of sedimentary grains. Compared with other pretreatment methods for size analysis of mudstones, this proposed method is more effective and has higher repeatability.

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

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.

Comparison of three different methods for effective introduction of platelet-rich plasma on PLGA woven mesh.

PubMed

Lee, Ji-Hye; Nam, Jinwoo; Kim, Hee Joong; Yoo, Jeong Joon

2015-03-11

For successful tissue regeneration, effective cell delivery to defect site is very important. Various types of polymer biomaterials have been developed and applied for effective cell delivery. PLGA (poly lactic-co-glycolic acid), a synthetic polymer, is a commercially available and FDA approved material. Platelet-rich plasma (PRP) is an autologous growth factor cocktail containing various growth factors including PDGF, TGFβ-1 and BMPs, and has shown positive effects on cell behaviors. We hypothesized that PRP pretreatment on PLGA mesh using different methods would cause different patterns of platelet adhesion and stages which would modulate cell adhesion and proliferation on the PLGA mesh. In this study, we pretreated PRP on PLGA using three different methods including simple dripping (SD), dynamic oscillation (DO) and centrifugation (CE), then observed the amount of adhered platelets and their activation stage distribution. The highest amount of platelets was observed on CE mesh and calcium treated CE mesh. Moreover, calcium addition after PRP coating triggered dramatic activation of platelets which showed large and flat morphologies of platelets with rich fibrin networks. Human chondrocytes (hCs) and human bone marrow stromal cells (hBMSCs) were next cultured on PRP-pretreated PLGA meshes using different preparation methods. CE mesh showed a significant increase in the initial cell adhesion of hCs and proliferation of hBMSCs compared with SD and DO meshes. The results demonstrated that the centrifugation method can be considered as a promising coating method to introduce PRP on PLGA polymeric material which could improve cell-material interaction using a simple method.

Physicochemical structural changes of poplar and switchgrass during biomass pretreatment and enzymatic hydrolysis

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

Meng, Xianzhi; Sun, Qining; Kosa, Matyas

Converting lignocellulosics to simple sugars for second generation bioethanol is complicated due to biomass recalcitrance, and it requires a pretreatment stage prior to enzymatic hydrolysis. In this study, native, pretreated (acid and alkaline) and partially hydrolyzed poplar and switchgrass were characterized by using Simons’ staining for cellulose accessibility, GPC for degree of polymerization (DP), and FTIR for chemical structure of plant cell wall. The susceptibility of the pretreated biomass to enzymatic hydrolysis could not be easily predicted from differences in cellulose DP and accessibility. During hydrolysis, the most significant DP reduction occurred at the very beginning of hydrolysis, and themore » DP began to decrease at a significantly slower rate after this initial period, suggesting an existence of a synergistic action of endo- and exoglucanases that contribute to the occurrence of a “peeling off” mechanism. Cellulose accessibility was found to be increased at the beginning of hydrolysis, after reaching a maximum value then started to decrease. In conclusion, the fresh enzyme restart hydrolysis experiment along with the accessibility data indicated that the factors associated with the nature of enzyme such as irreversible nonspecific binding of cellulases by lignin and steric hindrance of enzymes should be responsible for the gradual slowing down of the reaction rate.« less

Physicochemical structural changes of poplar and switchgrass during biomass pretreatment and enzymatic hydrolysis

DOE PAGES

Meng, Xianzhi; Sun, Qining; Kosa, Matyas; ...

2016-07-27

Converting lignocellulosics to simple sugars for second generation bioethanol is complicated due to biomass recalcitrance, and it requires a pretreatment stage prior to enzymatic hydrolysis. In this study, native, pretreated (acid and alkaline) and partially hydrolyzed poplar and switchgrass were characterized by using Simons’ staining for cellulose accessibility, GPC for degree of polymerization (DP), and FTIR for chemical structure of plant cell wall. The susceptibility of the pretreated biomass to enzymatic hydrolysis could not be easily predicted from differences in cellulose DP and accessibility. During hydrolysis, the most significant DP reduction occurred at the very beginning of hydrolysis, and themore » DP began to decrease at a significantly slower rate after this initial period, suggesting an existence of a synergistic action of endo- and exoglucanases that contribute to the occurrence of a “peeling off” mechanism. Cellulose accessibility was found to be increased at the beginning of hydrolysis, after reaching a maximum value then started to decrease. In conclusion, the fresh enzyme restart hydrolysis experiment along with the accessibility data indicated that the factors associated with the nature of enzyme such as irreversible nonspecific binding of cellulases by lignin and steric hindrance of enzymes should be responsible for the gradual slowing down of the reaction rate.« less

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.

Microneedle pretreatment enhances the percutaneous permeation of hydrophilic compounds with high melting points

PubMed Central

2012-01-01

Background Two commercially available microneedle rollers with a needle length of 200 μm and 300 μm were selected to examine the influence of microneedle pretreatment on the percutaneous permeation of four non-steroidal anti-inflammatory drugs (diclofenac, ibuprofen, ketoprofen, paracetamol) with different physicochemical drug characteristics in Franz-type diffusion cells. Samples of the receptor fluids were taken at predefined times over 6 hours and were analysed by UV–VIS high-performance liquid-chromatography. Histological examinations after methylene blue application were additionally performed to gather information about barrier disruption. Results Despite no visible pores in the stratum corneum, the microneedle pretreatment resulted in a twofold (200 μm) and threefold higher (300 μm) flux through the pretreated skin samples compared to untreated skin samples for ibuprofen and ketoprofen (LogKow > 3, melting point < 100°C). The flux of the hydrophilic compounds diclofenac and paracetamol (logKow < 1, melting point > 100°C) increased their amount by four (200 μm) to eight (300 μm), respectively. Conclusion Commercially available microneedle rollers with 200–300 μm long needles enhance the drug delivery of topically applied non-steroidal anti-inflammatory drugs and represent a valuable tool for percutaneous permeation enhancement particularly for substances with poor permeability due to a hydrophilic nature and high melting points. PMID:22947102

Design and performance of a new continuous-flow sample-introduction system for flame infrared-emission spectrometry: Applications in process analysis, flow injection analysis, and ion-exchange high-performance liquid chromatography.

PubMed

Lam, C K; Zhang, Y; Busch, M A; Busch, K W

1993-06-01

A new sample introduction system for the analysis of continuously flowing liquid streams by flame infrared-emission (FIRE) spectrometry has been developed. The system uses a specially designed purge cell to strip dissolved CO(2) from solution into a hydrogen gas stream that serves as the fuel for a hydrogen/air flame. Vibrationally excited CO(2) molecules present in the flame are monitored with a simple infrared filter (4.4 mum) photometer. The new system can be used to introduce analytes as a continuous liquid stream (process analysis mode) or on a discrete basis by sample injection (flow injection analysis mode). The key to the success of the method is the new purge-cell design. The small internal volume of the cell minimizes problems associated with purge-cell clean-out and produces sharp, reproducible signals. Spent analytical solution is continuously drained from the cell, making cell disconnection and cleaning between samples unnecessary. Under the conditions employed in this study, samples could be analyzed at a maximum rate of approximately 60/h. The new sample introduction system was successfully tested in both a process analysis- and a flow injection analysis mode for the determination of total inorganic carbon in Waco tap water. For the first time, flame infrared-emission spectrometry was successfully extended to non-volatile organic compounds by using chemical pretreatment with peroxydisulfate in the presence of silver ion to convert the analytes into dissolved carbon dioxide, prior to purging and detection by the FIRE radiometer. A test of the peroxydisulfate/Ag(+) reaction using six organic acids and five sugars indicated that all 11 compounds were oxidized to nearly the same extent. Finally, the new sample introduction system was used in conjunction with a simple filter FIRE radiometer as a detection system in ion-exchange high-performance liquid chromatography. Ion-exchange chromatograms are shown for two aqueous mixtures, one containing six organic acids and the second containing six mono-, di-, and trisaccharides.

Optical biosensor system with integrated microfluidic sample preparation and TIRF based detection

NASA Astrophysics Data System (ADS)

Gilli, Eduard; Scheicher, Sylvia R.; Suppan, Michael; Pichler, Heinz; Rumpler, Markus; Satzinger, Valentin; Palfinger, Christian; Reil, Frank; Hajnsek, Martin; Köstler, Stefan

2013-05-01

There is a steadily growing demand for miniaturized bioanalytical devices allowing for on-site or point-of-care detection of biomolecules or pathogens in applications like diagnostics, food testing, or environmental monitoring. These, so called labs-on-a-chip or micro-total analysis systems (μ-TAS) should ideally enable convenient sample-in - result-out type operation. Therefore, the entire process from sample preparation, metering, reagent incubation, etc. to detection should be performed on a single disposable device (on-chip). In the early days such devices were mainly fabricated using glass or silicon substrates and adapting established fabrication technologies from the electronics and semiconductor industry. More recently, the development focuses on the use of thermoplastic polymers as they allow for low-cost high volume fabrication of disposables. One of the most promising materials for the development of plastic based lab-on-achip systems are cyclic olefin polymers and copolymers (COP/COC) due to their excellent optical properties (high transparency and low autofluorescence) and ease of processing. We present a bioanalytical system for whole blood samples comprising a disposable plastic chip based on TIRF (total internal reflection fluorescence) optical detection. The chips were fabricated by compression moulding of COP and microfluidic channels were structured by hot embossing. These microfluidic structures integrate several sample pretreatment steps. These are the separation of erythrocytes, metering of sample volume using passive valves, and reagent incubation for competitive bioassays. The surface of the following optical detection zone is functionalized with specific capture probes in an array format. The plastic chips comprise dedicated structures for simple and effective coupling of excitation light from low-cost laser diodes. This enables TIRF excitation of fluorescently labeled probes selectively bound to detection spots at the microchannel surface. The fluorescence of these detection arrays is imaged using a simple set-up based on a digital consumer camera. Image processing for spot detection and intensity calculation is accomplished using customized software. Using this combined TIRF excitation and imaging based detection approach allowes for effective suppression of background fluorescence from the sample, multiplexed detection in an array format, as well as internal calibration and background correction.

Procedure for rapid determination of δ15N and δ18O values of nitrate: development and application to an irrigated rice paddy watershed.

PubMed

Yada, Saeko; Nakajima, Yasuhiro; Itahashi, Sunao; Asada, Kei; Yoshikawa, Seiko; Eguchi, Sadao

2016-01-01

The dual isotope approach using the stable isotope ratios of nitrate nitrogen (δ(15)N(NO3)) and oxygen (δ(18)O(NO3)) is a strong tool for identifying the history of nitrate in various environments. Basically, a rapid procedure for determining δ(15)N(NO3) and δ(18)O(NO3) values is required to analyze many more samples quickly and thus save on the operational costs of isotope-ratio mass spectrometry (IRMS). We developed a new rapid procedure to save time by pre-treating consecutive samples of nitrous oxide microbially converted from nitrate before IRMS determination. By controlling two six-port valves of the pre-treatment system separately, IRMS determination of the current sample and backflush during the next sample pre-treatment period could be conducted simultaneously. A set of 89 samples was analyzed precisely during a 25-h continuous run (17 min per sample), giving the fastest reported processing time, and simultaneously reducing liquid nitrogen and carrier helium gas consumption by 35%. Application of the procedure to an irrigated rice paddy watershed suggested that nitrate concentrations in river waters decreased in a downstream direction, mainly because of the mixing of nitrate from different sources, without distinct evidence of denitrification. Our procedure should help with more detailed studies of nitrate formation processes in watersheds.

CZE determination of submicromolar level of phenol in seawater using improved dynamic pH junction.

PubMed

Yasuno, Koki; Fukushi, Keiichi

2016-10-01

Using an improved dynamic pH junction as an on-line concentration procedure, we developed CZE for determining submicromolar phenol in seawater for chloride to phenol concentration ratios of 1 000 000. To enhance the effect of conventional dynamic pH junction, a saturated fatty acid solution was injected into the capillary after sample injection. We named the procedure an improved dynamic pH junction. The method requires no sample pretreatment. The following optimum conditions were established: BGE, 40 mM sodium tetraborate decahydrate adjusted to pH 9.8 containing 0.001% m/v hexadimethrine bromide; 190 nm detection wavelength; 18 s (370 nL) vacuum injection period of sample; a saturated fatty acid solution, 30 mM sodium n-hexanoate; 20 s (420 nL) vacuum injection period of the sodium n-hexanoate; and 15 kV applied voltage with the sample inlet side as the cathode. The LOD for phenol was 5.9 μg/L at S/N of 3. The respective values of the RSD (intraday) of the peak area, peak height, and migration time for phenol were 1.9, 2.9, and 0.46%. The recoveries of phenol (25-100 μg/L) spiked into the natural seawater sample obtained using the peak areas were 92-110%. The proposed method was applied to simple biodegradation experiments using natural seawater samples containing phenol. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of pretreatment with epoxy compounds on the mechanical properties of bovine pericardial bioprosthetic materials.

PubMed

Xi, T; Liu, F; Xi, B

1992-07-01

Early failures of bovine pericardial heart valves are due to leaflet perforation, tearing and calcification. Since glutaraldehyde fixation has been shown to produce marked changes in leaflet mechanics and has been linked to development of calcification, bovine pericardium fixed with the four hydrophilic epoxy formulations and their mechanical properties are studied in this paper. We measured the thicknesses, shrinkage temperatures, stress relaxations and stress-strain curves of bovine pericardiums after different treatments with (1) non-treatment (fresh), (2) glutaraldehyde (GA), (3) epoxy compounds followed by the posttreatment with GA (EP 1#, EP 2#), and (4) epoxy compounds (EP 3# and EP 4#). Results of this study showed that the hydrophilic epoxy compounds are good crosslinking agents. There are no significant differences of shrinkage temperature and ultimate tensile stress among all tissue samples pretreated with GA, EP 1# and EP 2#. However, the stress relaxations of tissue-samples pretreated with epoxy compounds followed by the posttreatment with GA (EP 1# and EP 2#) are significantly slower than that pretreated with GA, and the strains at fracture of EP 1# and EP 2# are also significantly larger than that of GA or epoxy compounds. These facts show that the bovine pericardium pretreated with the epoxy compound followed by the posttreatment with GA (EP 1# and EP 2#) possesses greater tenacity and potential durability in dynamic stress.

Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid micro-volume samples

PubMed Central

Schaper, J. Niklas; Pfeuffer, Kevin P.; Shelley, Jacob T.; Bings, Nicolas H.

2012-01-01

One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads can quench the afterglow and, thus, the formation of reagent ions. As a result, the analysis of liquid samples is preferably carried out by analyzing dried residues or by desorbing small amounts of liquid samples directly from the liquid surface. In the former case, reproducibility of sample introduction is crucial if quantitative results are desired. In the present study, introduction of liquid samples as very small droplets helps overcome the issues of sample positioning and reduced levels of solvent intake. A recently developed “drop-on-demand” (DOD) aerosol generator is capable of reproducibly producing very small volumes of liquid (~17 pL). In this paper, the coupling of FAPA-MS and DOD is reported and applications are suggested. Analytes representing different classes of substances were tested and limits of detections were determined. Matrix tolerance was investigated for drugs of abuse and their metabolites by analyzing raw urine samples and quantification without the use of internal standards. Limits of detection below 2 µg/mL, without sample pretreatment, were obtained. PMID:23025277

Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid microvolume samples.

PubMed

Schaper, J Niklas; Pfeuffer, Kevin P; Shelley, Jacob T; Bings, Nicolas H; Hieftje, Gary M

2012-11-06

One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads can quench the afterglow and, thus, the formation of reagent ions. As a result, the analysis of liquid samples is preferably carried out by analyzing dried residues or by desorbing small amounts of liquid samples directly from the liquid surface. In the former case, reproducibility of sample introduction is crucial if quantitative results are desired. In the present study, introduction of liquid samples as very small droplets helps overcome the issues of sample positioning and reduced levels of solvent intake. A recently developed "drop-on-demand" (DOD) aerosol generator is capable of reproducibly producing very small volumes of liquid (∼17 pL). In this paper, the coupling of FAPA-MS and DOD is reported and applications are suggested. Analytes representing different classes of substances were tested and limits of detections were determined. Matrix tolerance was investigated for drugs of abuse and their metabolites by analyzing raw urine samples and quantification without the use of internal standards. Limits of detection below 2 μg/mL, without sample pretreatment, were obtained.

Effects of alprazolam on capture stress-related serum cortisol responses in Korean raccoon dogs (Nyctereutes procyonoides koreensis)

PubMed Central

Kim, Sun-A; Lee, So-Yeong; Kimura, Junpei

2011-01-01

The purpose of this study was to evaluate the effect of alprazolam on the stress that Korean raccoon dogs (Nyctereutes procyonoides koreensis) may experience while caught in a live trap by measuring their serum cortisol response. The animals were placed in a live trap with or without being pretreated with oral doses of alprazolam. In both groups, pre-trap blood samples were initially collected without anesthesia before the animals were positioned in the live trap; then post-trap blood samples were collected after the animals had remained in the live trap for 2 h. Changes in cortisol levels were observed using a chemiluminescent immunoassay. The level of cortisol increased in the control group and decreased in the alprazolam-pretreatment group (p < 0.05). In this study, we demonstrated that alprazolam pretreatment reduced stress during live trap capture. PMID:21368571

Effects of alprazolam on capture stress-related serum cortisol responses in Korean raccoon dogs (Nyctereutes procyonoides koreensis).

PubMed

Kim, Sun-A; Lee, So-Yeong; Kimura, Junpei; Shin, Nam-Shik

2011-03-01

The purpose of this study was to evaluate the effect of alprazolam on the stress that Korean raccoon dogs (Nyctereutes procyonoides koreensis) may experience while caught in a live trap by measuring their serum cortisol response. The animals were placed in a live trap with or without being pretreated with oral doses of alprazolam. In both groups, pre-trap blood samples were initially collected without anesthesia before the animals were positioned in the live trap; then post-trap blood samples were collected after the animals had remained in the live trap for 2 h. Changes in cortisol levels were observed using a chemiluminescent immunoassay. The level of cortisol increased in the control group and decreased in the alprazolam-pretreatment group (p < 0.05). In this study, we demonstrated that alprazolam pretreatment reduced stress during live trap capture.

Biotechnological application of sustainable biogas production through dry anaerobic digestion of Napier grass.

PubMed

Dussadee, Natthawud; Ramaraj, Rameshprabu; Cheunbarn, Tapana

2017-05-01

Napier grass (Pennisetum purpureum), represents an interesting substrate for biogas production. The research project evaluated biogas potential production from dry anaerobic digestion of Napier grass using batch experiment. To enhance the biogas production from ensiled Napier grass, thermal and alkaline pre-treatments were performed in batch mode. Alkali hydrolysis of Napier grass was performed prior to batch dry anaerobic digestion at three different mild concentrations of sodium hydroxide (NaOH). The study results confirmed that NaOH pretreated sample produced high yield of biogas than untreated (raw) and hot water pretreated samples. Napier grass was used as the mono-substrate. The biogas composition of carbon dioxide (30.10%), methane (63.50%) and 5 ppm of H 2 S was estimated from the biogas. Therefore, fast-growing, high-yielding and organic matter-enriched of Napier grass was promising energy crop for biogas production.

Evaluation of efficient glucose release using sodium hydroxide and phosphoric acid as pretreating agents from the biomass of Sesbania grandiflora (L.) Pers.: A fast growing tree legume.

PubMed

Mund, Nitesh K; Dash, Debabrata; Barik, Chitta R; Goud, Vaibhav V; Sahoo, Lingaraj; Mishra, Prasannajit; Nayak, Nihar R

2017-07-01

Sesbania grandiflora (L.) Pers. is one of the fast growing tree legumes having the efficiency to produce around 50tha -1 above ground dry matters in a year. In this study, biomass of 2years old S. grandiflora was selected for the chemical composition, pretreatments and enzymatic hydrolysis studies. The stem biomass with a wood density of 3.89±0.01gmcm -3 contains about 38% cellulose, 12% hemicellulose and 28% lignin. Enzymatic hydrolysis of pretreated biomass revealed that phosphoric acid (H 3 PO 4 ) pretreated samples even at lower cellulase loadings [1 Filter Paper Units (FPU)], could efficiently convert about 86% glucose, while, even at higher cellulase loadings (60FPU) alkali pretreated biomass could convert only about 58% glucose. The effectiveness of phosphoric acid pretreatment was also supported by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and Fourier transform infrared spectroscopy (FTIR) analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Complex effect of lignocellulosic biomass pretreatment with 1-butyl-3-methylimidazolium chloride ionic liquid on various aspects of ethanol and fumaric acid production by immobilized cells within SSF.

PubMed

Dotsenko, Anna S; Dotsenko, Gleb S; Senko, Olga V; Stepanov, Nikolay A; Lyagin, Ilya V; Efremenko, Elena N; Gusakov, Alexander V; Zorov, Ivan N; Rubtsova, Ekaterina A

2018-02-01

The pretreatment of softwood and hardwood samples (spruce and hornbeam wood) with 1-butyl-3-methylimidazolium chloride ([Bmim]Cl) was undertaken for further simultaneous enzymatic saccharification of renewable non-food lignocellulosic biomass and microbial fermentation of obtained sugars to ethanol and fumaric acid. A multienzyme cocktail based on cellulases and yeast or fungus cells producing ethanol and fumaric acid were the main objects of [Bmim]Cl influence studies. A complex effect of lignocellulosic biomass pretreatment with [Bmim]Cl on various aspects of the process (both action of cellulases and microbial conversion of hydrolysates to target products) was revealed. Positive effects of the pretreatment with [Bmim]Cl included decreasing the lignin content in the biomass, and increasing the effectiveness of enzymatic hydrolysis and microbial transformation of pretreated biomass. Immobilized cells of both yeasts and fungi possessed improved productive characteristics in the biotransformation of biomass pretreated with [Bmim]Cl to ethanol and fumaric acid. Copyright © 2017 Elsevier Ltd. All rights reserved.

Cellulose pretreatment with 1-n-butyl-3-methylimidazolium chloride for solid acid-catalyzed hydrolysis.

PubMed

Kim, Soo-Jin; Dwiatmoko, Adid Adep; Choi, Jae Wook; Suh, Young-Woong; Suh, Dong Jin; Oh, Moonhyun

2010-11-01

This study has been focused on developing a cellulose pretreatment process using 1-n-butyl-3-methylimidazolium chloride ([bmim]Cl) for subsequent hydrolysis over Nafion(R) NR50. Thus, several pretreatment variables such as the pretreatment period and temperature, and the [bmim]Cl amount were varied. Additionally, the [bmim]Cl-treated cellulose samples were characterized by X-ray diffraction analysis, and their crystallinity index values including CI(XD), CI(XD-CI) and CI(XD-CII) were then calculated. When correlated with these values, the concentrations of total reducing sugars (TRS) obtained by the pretreatment of native cellulose (NC) and glucose produced by the hydrolysis reaction were found to show a distinct relationship with the [CI(NC)-CI(XD)] and CI(XD-CII) values, respectively. Consequently, the cellulose pretreatment step with [bmim]Cl is to loosen a crystalline cellulose through partial transformation of cellulose I to cellulose II and, furthermore, the TRS release, while the subsequent hydrolysis of [bmim]Cl-treated cellulose over Nafion(R) NR50 is effective to convert cellulose II to glucose. Copyright 2010 Elsevier Ltd. All rights reserved.

The correlation between cellulose allomorphs (I and II) and conversion after removal of hemicellulose and lignin of lignocellulose.

PubMed

Song, Yanliang; Zhang, Jingzhi; Zhang, Xu; Tan, Tianwei

2015-10-01

H2SO4, NaOH and H3PO4 were applied to decompose lignocellulose samples (giant reeds, pennisetum and cotton stalks) to investigate the correlation between cellulose allomorphs (cellulose I and II) and conversion of cellulose. The effect of removal of hemicellulose and lignin on the surface morphology, crystallinity index (CrI), cellulose allomorphs (cellulose I and II), and enzymatic hydrolysis under different pretreatments was also studied. CrI caused by H3PO4 pretreatment reached 11.19%, 24.93% and 8.15% for the three samples, respectively. Corn stalk showed highest conversion of cellulose among three samples, irrespective of the pretreatment used. This accounted for the widely use of corn stalk as the renewable crop substrate to synthesize biofuels like ethanol. CrI of cellulose I (CrI-I) negatively affects cellulose conversion but CrI of cellulose II (CrI-II) positively affects cellulose conversion. It contributes to make the strategy to transform cellulose I to cellulose II and enhancing enzymatic hydrolysis of lignocellulose. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

FIELD-SCALE STUDIES: HOW DOES SOIL SAMPLE PRETREATMENT AFFECT REPRESENTATIVENESS ? (ABSTRACT)

EPA Science Inventory

Samples from field-scale studies are very heterogeneous and can contain large soil and rock particles. Oversize materials are often removed before chemical analysis of the soil samples because it is not practical to include these materials. Is the extracted sample representativ...

FIELD-SCALE STUDIES: HOW DOES SOIL SAMPLE PRETREATMENT AFFECT REPRESENTATIVENESS?

EPA Science Inventory

Samples from field-scale studies are very heterogeneous and can contain large soil and rock particles. Oversize materials are often removed before chemical analysis of the soil samples because it is not practical to include these materials. Is the extracted sample representativ...

Development of a Rapid LC-MS/MS Method for the Determination of Emerging Fusarium mycotoxins Enniatins and Beauvericin in Human Biological Fluids

PubMed Central

Serrano, Ana Belén; Capriotti, Anna Laura; Cavaliere, Chiara; Piovesana, Susy; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

2015-01-01

A novel method for the simultaneous determination of enniatins A, A1, B and B1 and beauvericin, both in human urine and plasma samples, was developed and validated. The method consisted of a simple and easy pretreatment, specific for each matrix, followed by solid phase extraction (SPE) and detection by high performance liquid chromatography-tandem mass spectrometry with an electrospray ion source. The optimized SPE method was performed on graphitized carbon black cartridges after suitable dilution of the extracts, which allowed high mycotoxin absolute recoveries (76%–103%) and the removal of the major interferences from the matrix. The method was extensively evaluated for plasma and urine samples separately, providing satisfactory results in terms of linearity (R2 of 0.991–0.999), process efficiency (>81%), trueness (recoveries between 85% and 120%), intra-day precision (relative standard deviation, RSD < 18%), inter-day precision (RSD < 21%) and method quantification limits (ranging between 20 ng·L−1 and 40 ng·L−1 in plasma and between 5 ng·L−1 and 20 ng·L−1 in urine). Finally, the highly sensitive validated method was applied to some urine and plasma samples from different donors. PMID:26371043

Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry.

PubMed

Hartmann, Georg; Schuster, Michael

2013-01-25

The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of moxifloxacin in human plasma, plasma ultrafiltrate, and cerebrospinal fluid by a rapid and simple liquid chromatography- tandem mass spectrometry method.

PubMed

Pranger, Arianna D; Alffenaar, Jan-Willem C; Wessels, A Mireille A; Greijdanus, Ben; Uges, Donald R A

2010-04-01

Moxifloxacin (MFX) is a useful agent in the treatment of multi-drug-resistant tuberculosis (MDR-TB). At Tuberculosis Centre Beatrixoord, a referral center for tuberculosis in the Netherlands, approximately 36% of the patients have received MFX as treatment. Based on the variability of MFX AUC, the variability of in vitro susceptibility to MFX of M. tuberculosis, and the variability of penetration into sanctuary sites, measuring the concentration of MFX in plasma and cerebrospinal fluid (CSF) could be recommended. Therefore, a rapid and validated liquid chromatography-tandem mass spectrometry (LC-MS-MS) analyzing method with a simple pretreatment procedure was developed for therapeutic drug monitoring of MFX in human plasma and CSF. Because of the potential influence of protein binding on efficacy, we decided to determine both bound and unbound (ultrafiltrate) fraction of MFX. The calibration curves were linear in the therapeutic range of 0.05 to 5.0 mg/L plasma and CSF with CV in the range of -5.4% to 9.3%. MFX ultrafiltrate samples could be determined with the same method setup for analysis of MFX in CSF. The LC-MS-MS method developed in this study is suitable for monitoring MFX in human plasma, plasma ultrafiltrate, and CSF.

Phosphate conversion coating reduces the degradation rate and suppresses side effects of metallic magnesium implants in an animal model.

PubMed

Rahim, Muhammad Imran; Tavares, Ana; Evertz, Florian; Kieke, Marc; Seitz, Jan-Marten; Eifler, Rainer; Weizbauer, Andreas; Willbold, Elmar; Jürgen Maier, Hans; Glasmacher, Birgit; Behrens, Peter; Hauser, Hansjörg; Mueller, Peter P

2017-08-01

Magnesium alloys have promising mechanical and biological properties for the development of degradable implants. However, rapid implant corrosion and gas accumulations in tissue impede clinical applications. With time, the implant degradation rate is reduced by a highly biocompatible, phosphate-containing corrosion layer. To circumvent initial side effects after implantation it was attempted to develop a simple in vitro procedure to generate a similarly protective phosphate corrosion layer. To this end magnesium samples were pre-incubated in phosphate solutions. The resulting coating was well adherent during routine handling procedures. It completely suppressed the initial burst of corrosion and it reduced the average in vitro magnesium degradation rate over 56 days almost two-fold. In a small animal model phosphate coatings on magnesium implants were highly biocompatible and abrogated the appearance of gas cavities in the tissue. After implantation, the phosphate coating was replaced by a layer with an elemental composition that was highly similar to the corrosion layer that had formed on plain magnesium implants. The data demonstrate that a simple pre-treatment could improve clinically relevant properties of magnesium-based implants. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 1622-1635, 2017. © 2016 Wiley Periodicals, Inc.

Pin-based electrochemical glucose sensor with multiplexing possibilities.

PubMed

Rama, Estefanía C; Costa-García, Agustín; Fernández-Abedul, M Teresa

2017-02-15

This work describes the use of mass-produced stainless-steel pins as low-cost electrodes to develop simple and portable amperometric glucose biosensors. A potentiostatic three-electrode configuration device is designed using two bare pins as reference and counter electrodes, and a carbon-ink coated pin as working electrode. Conventional transparency film without any pretreatment is used to punch the pins and contain the measurement solution. The interface to the potentiostat is very simple since it is based on a commercial female connection. This electrochemical system is applied to glucose determination using a bienzymatic sensor phase (glucose oxidase/horseradish peroxidase) with ferrocyanide as electron-transfer mediator, achieving a linear range from 0.05 to 1mM. It shows analytical characteristics comparable to glucose sensors previously reported using conventional electrodes, and its application for real food samples provides good results. The easy modification of the position of the pins allows designing different configurations with possibility of performing simultaneous measurements. This is demonstrated through a specific design that includes four pin working-electrodes. Different concentrations of antibody labeled with alkaline phosphatase are immobilized on the pin-heads and after enzymatic conversion of 3-indoxylphosphate and silver nitrate, metallic silver is determined by anodic stripping voltammetry. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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

The effect of acid hydrolysis pretreatment on crystallinity and solubility of kenaf cellulose membrane

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

Saidi, Anis Syuhada Mohd; Zakaria, Sarani; Chia, Chin Hua

2015-09-25

Cellulose was extracted from kenaf core pulp (KCP) by series of bleaching steps in the sequence (DEED) where D and E are referred as acid and alkali treatment. The bleached kenaf pulp (BKCP) is then pretreated with acid hydrolysis at room temperature for 1 and 3 h respectively. The pretreated cellulose is dissolved in lithium hydroxide/urea (LiOH/urea) and cellulose solution produced was immersed in distilled water bath. BKCP without treatment was also conducted for comparison purpose. The effects of acid hydrolysis pretreatment on solubility and crystallinity are investigated. Higher solubility of cellulose solution is achieved for treated samples. Cellulose II formationmore » and crystallinity index of the cellulose membrane were determined by X-ray diffraction (XRD)« less

Thermophilic bio-hydrogen production from corn-bran residue pretreated by calcined-lime mud from papermaking process.

PubMed

Zhang, Jishi; Zhang, Junjie; Zang, Lihua

2015-12-01

This study investigated the use of calcined-lime mud from papermaking process (CLMP) pretreatment to improve fermentative hydrogen yields from corn-bran residue (CBR). CBR samples were pretreated with different concentrations (0-15 g/L) of CLMP at 55°C for 48 h, prior to the thermophilic fermentation with heat-treated anaerobic sludge inoculum. The maximum hydrogen yield (MHY) of 338.91 ml/g-VS was produced from the CBR pretreated with 10 g/L CLMP, with the corresponding lag-phase time of 8.24h. Hydrogen yield increments increased from 27.76% to 48.07%, compared to the control. The CLMP hydrolyzed more cellulose, which provided adequate substrates for hydrogen production. Copyright © 2015 Elsevier Ltd. All rights reserved.

A colorimetric probe based on desensitized ionene-stabilized gold nanoparticles for single-step test for sulfate ions.

PubMed

Arkhipova, Viktoriya V; Apyari, Vladimir V; Dmitrienko, Stanislava G

2015-03-15

Desensitized ionene-stabilized gold nanoparticles have been prepared and applied as a colorimetric probe for the single-step test for sulfate ions at the relatively high concentration level. The approach is based on aggregation of the nanoparticles leading to the change in absorption spectra and color of the solution. These nanoparticles are characterized by the decreased sensitivity due to both electrostatic and steric stabilization, which allows for simple, and rapid direct single-step determination of sulfate at the relatively high concentration level in real water samples without sample pretreatment or dilution. Influence of different factors (the time of interaction, pH, the concentrations of sulfate ions and the nanoparticles) on the aggregation and analytical performance of the procedure was investigated. The method allows for the determination of sulfate ions in the mass range of 0.2-0.4 mg with RSD of 5% from the sample volume of less than 2 mL. It has a sharp dependence of the colorimetric response on the concentration of sulfate, which makes it prospective for indicating deviations of the sulfate concentration regarding some declared value chosen within the above range. The time of the analysis is 2 min. The method was applied to the analysis of mineral water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Multi-walled carbon nanotubes-dispersive solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for the analysis of 18 sulfonamides in pork.

PubMed

Hou, Xiao-Lin; Wu, Yin-Liang; Yang, Ting; Du, Xiang-Dang

2013-06-15

A simple and cost-effective pre-treatment procedure was developed for 18 sulfonamides in pork using dispersive solid phase extraction (dSPE) with multi-walled carbon nanotubes (MWCNTs). The sample was analysed after purification by ultra high-performance liquid chromatography-positive electrospray ionisation tandem mass spectrometry (UHPLC-ESI-MS/MS). After extraction with phosphate buffer (pH 6.0), a dSPE procedure was conducted with MWCNTs. The pH value of the extract, extraction time with MWCNTs, type and amount of MWCNTs and type of eluent were optimised to increase the sample throughput and sensitivity. The samples were quantified using sulfamethazine-(13)C6 as an internal standard. The recoveries of the target compounds from the pork samples were most efficient when 150mg of MWCNTs with an outer diameter of less than 8nm and a length of 0.5-2μm was used. A mixture of acetonitrile/50mM ammonium acetate (95:5, v/v) was shown to be the most suitable solvent for desorbing the compounds from the MWCNTs. The proposed method was validated according to the European Commission Decision 2002/657/EC, which determines linearity, specificity, decision limit (CCα), detection capability (CCβ), recovery, precision and stability. Copyright © 2013 Elsevier B.V. All rights reserved.

Improvement of the enzymatic hydrolysis of furfural residues by pretreatment with combined green liquor and hydrogen peroxide.

PubMed

Yu, Hai-Long; Tang, Yong; Xing, Yang; Zhu, Li-Wei; Jiang, Jian-Xin

2013-11-01

A potential commercial pretreatment for furfural residues (FRs) was investigated by using a combination of green liquor and hydrogen peroxide (GL-H2O2). The results showed that 56.2% of lignin removal was achieved when the sample was treated with 0.6 g H2O2/g-DS (dry substrate) and 6 mL GL/g-DS at 80 °C for 3 h. After 96 h hydrolysis with 18 FPU/g-cellulose for cellulase, 27 CBU/g-cellulose for β-glucosidase, the glucose yield increased from 71.2% to 83.6%. Ethylenediaminetetraacetic acid was used to reduce the degradation of H2O2, the glucose yield increased to 90.4% after the addition of 1% (w/w). The untreated FRs could bind more easily to cellulase than pretreated FRs could. The structural changes on the surface of sample were characterized by X-ray photoelectron spectroscopy. The results indicated that the surface lignin could be effectively removed during pretreatment, thereby decreasing the enzyme-lignin binding activity. Moreover, the carbonyl from lignin plays an important role in cellulase binding. Copyright © 2013 Elsevier Ltd. All rights reserved.

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.

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.

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.

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.

Spectral identification of melon seeds variety based on k-nearest neighbor and Fisher discriminant analysis

NASA Astrophysics Data System (ADS)

Li, Cuiling; Jiang, Kai; Zhao, Xueguan; Fan, Pengfei; Wang, Xiu; Liu, Chuan

2017-10-01

Impurity of melon seeds variety will cause reductions of melon production and economic benefits of farmers, this research aimed to adopt spectral technology combined with chemometrics methods to identify melon seeds variety. Melon seeds whose varieties were "Yi Te Bai", "Yi Te Jin", "Jing Mi NO.7", "Jing Mi NO.11" and " Yi Li Sha Bai "were used as research samples. A simple spectral system was developed to collect reflective spectral data of melon seeds, including a light source unit, a spectral data acquisition unit and a data processing unit, the detection wavelength range of this system was 200-1100nm with spectral resolution of 0.14 7.7nm. The original reflective spectral data was pre-treated with de-trend (DT), multiple scattering correction (MSC), first derivative (FD), normalization (NOR) and Savitzky-Golay (SG) convolution smoothing methods. Principal Component Analysis (PCA) method was adopted to reduce the dimensions of reflective spectral data and extract principal components. K-nearest neighbour (KNN) and Fisher discriminant analysis (FDA) methods were used to develop discriminant models of melon seeds variety based on PCA. Spectral data pretreatments improved the discriminant effects of KNN and FDA, FDA generated better discriminant results than KNN, both KNN and FDA methods produced discriminant accuracies reaching to 90.0% for validation set. Research results showed that using spectral technology in combination with KNN and FDA modelling methods to identify melon seeds variety was feasible.

Evaluation of the Persistence of Infectious Human Noroviruses on Food Surfaces by Using Real-Time Nucleic Acid Sequence-Based Amplification▿

PubMed Central

Lamhoujeb, Safaa; Fliss, Ismail; Ngazoa, Solange E.; Jean, Julie

2008-01-01

Noroviruses (NoV) are the major cause of nonbacterial gastroenteritis. However, there is no published study to ascertain their survival on foodstuffs which are directly related to human health risk. In the present study, we developed a rapid, simple, and sensitive real-time nucleic acid sequence-based amplification (NASBA) combined with an enzymatic treatment for distinguishing infectious from noninfectious human NoV. The developed method was validated using spiked ready-to-eat food samples. When feline calicivirus (FCV) was used as a NoV surrogate in the preliminary assays, it appeared more sensitive to heat inactivation and enzymatic pretreatment than the human NoV. This suggests that FCV may not be an ideal model for studying NoV. Our results reveal clearly that the developed enzymatic pretreatment/real-time NASBA combination successfully distinguished the infectious from heat-inactivated NoV. Moreover, we demonstrate that NoV survived for at least 10 days on refrigerated ready-to-eat foods, such as lettuce and turkey. However, the survival rate was higher on turkey than on lettuce, probably because of their different surface natures. The approach developed in this study may be suitable for more in-depth studies of the persistence and inactivation of human NoV and may be applied to other nonculturable RNA viruses. Moreover, the evaluation of infectious NoV survival provided valuable information concerning its persistence on ready-to-eat food. PMID:18378643

Rapid and Specific Detection of Salmonella spp. in Animal Feed Samples by PCR after Culture Enrichment

PubMed Central

Löfström, Charlotta; Knutsson, Rickard; Axelsson, Charlotta Engdahl; Rådström, Peter

2004-01-01

A PCR procedure has been developed for routine analysis of viable Salmonella spp. in feed samples. The objective was to develop a simple PCR-compatible enrichment procedure to enable DNA amplification without any sample pretreatment such as DNA extraction or cell lysis. PCR inhibition by 14 different feed samples and natural background flora was circumvented by the use of the DNA polymerase Tth. This DNA polymerase was found to exhibit a high level of resistance to PCR inhibitors present in these feed samples compared to DyNAzyme II, FastStart Taq, Platinum Taq, Pwo, rTth, Taq, and Tfl. The specificity of the Tth assay was confirmed by testing 101 Salmonella and 43 non-Salmonella strains isolated from feed and food samples. A sample preparation method based on culture enrichment in buffered peptone water and DNA amplification with Tth DNA polymerase was developed. The probability of detecting small numbers of salmonellae in feed, in the presence of natural background flora, was accurately determined and found to follow a logistic regression model. From this model, the probability of detecting 1 CFU per 25 g of feed in artificially contaminated soy samples was calculated and found to be 0.81. The PCR protocol was evaluated on 155 naturally contaminated feed samples and compared to an established culture-based method, NMKL-71. Eight percent of the samples were positive by PCR, compared with 3% with the conventional method. The reasons for the differences in sensitivity are discussed. Use of this method in the routine analysis of animal feed samples would improve safety in the food chain. PMID:14711627

Online residence time distribution measurement of thermochemical biomass pretreatment reactors

DOE PAGES

Sievers, David A.; Kuhn, Erik M.; Stickel, Jonathan J.; ...

2015-11-03

Residence time is a critical parameter that strongly affects the product profile and overall yield achieved from thermochemical pretreatment of lignocellulosic biomass during production of liquid transportation fuels. The residence time distribution (RTD) is one important measure of reactor performance and provides a metric to use when evaluating changes in reactor design and operating parameters. An inexpensive and rapid RTD measurement technique was developed to measure the residence time characteristics in biomass pretreatment reactors and similar equipment processing wet-granular slurries. Sodium chloride was pulsed into the feed entering a 600 kg/d pilot-scale reactor operated at various conditions, and aqueous saltmore » concentration was measured in the discharge using specially fabricated electrical conductivity instrumentation. This online conductivity method was superior in both measurement accuracy and resource requirements compared to offline analysis. Experimentally measured mean residence time values were longer than estimated by simple calculation and screw speed and throughput rate were investigated as contributing factors. In conclusion, a semi-empirical model was developed to predict the mean residence time as a function of operating parameters and enabled improved agreement.« less

Fermentative hydrogen production using pretreated microalgal biomass as feedstock.

PubMed

Wang, Jianlong; Yin, Yanan

2018-02-14

Microalgae are simple chlorophyll containing organisms, they have high photosynthetic efficiency and can synthesize and accumulate large quantities of carbohydrate biomass. They can be cultivated in fresh water, seawater and wastewater. They have been used as feedstock for producing biodiesel, bioethanol and biogas. The production of these biofuels can be integrated with CO 2 mitigation, wastewater treatment, and the production of high-value chemicals. Biohydrogen from microalgae is renewable. Microalgae have several advantages compared to terrestrial plants, such as higher growth rate with superior CO 2 fixation capacity; they do not need arable land to grow; they do not contain lignin. In this review, the biology of microalgae and the chemical composition of microalgae were briefly introduced, the advantages and disadvantages of hydrogen production from microalgae were discussed, and the pretreatment of microalgal biomass and the fermentative hydrogen production from microalgal biomass pretreated by different methods (including physical, chemical, biological and combined methods) were summarized and evaluated. For the production of biohydrogen from microalgae, the economic feasibility remains the most important aspect to consider. Several technological and economic issues must be addressed to achieve success on a commercial scale.

Floating Chip Mounting System Driven by Repulsive Force of Permanent Magnets for Multiple On-Site SPR Immunoassay Measurements

PubMed Central

Horiuchi, Tsutomu; Tobita, Tatsuya; Miura, Toru; Iwasaki, Yuzuru; Seyama, Michiko; Inoue, Suzuyo; Takahashi, Jun-ichi; Haga, Tsuneyuki; Tamechika, Emi

2012-01-01

We have developed a measurement chip installation/removal mechanism for a surface plasmon resonance (SPR) immunoassay analysis instrument designed for frequent testing, which requires a rapid and easy technique for changing chips. The key components of the mechanism are refractive index matching gel coated on the rear of the SPR chip and a float that presses the chip down. The refractive index matching gel made it possible to optically couple the chip and the prism of the SPR instrument easily via elastic deformation with no air bubbles. The float has an autonomous attitude control function that keeps the chip parallel in relation to the SPR instrument by employing the repulsive force of permanent magnets between the float and a float guide located in the SPR instrument. This function is realized by balancing the upward elastic force of the gel and the downward force of the float, which experiences a leveling force from the float guide. This system makes it possible to start an SPR measurement immediately after chip installation and to remove the chip immediately after the measurement with a simple and easy method that does not require any fine adjustment. Our sensor chip, which we installed using this mounting system, successfully performed an immunoassay measurement on a model antigen (spiked human-IgG) in a model real sample (non-homogenized milk) that included many kinds of interfering foreign substances without any sample pre-treatment. The ease of the chip installation/removal operation and simple measurement procedure are suitable for frequent on-site agricultural, environmental and medical testing. PMID:23202030

Ultrasonication followed by single-drop microextraction combined with GC/MS for rapid determination of organochlorine pesticides from fish.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2008-02-01

A novel, rapid and simple sample pretreatment technique termed ultrasonication followed by single-drop micro-extraction (U-SDME) has been developed and combined with GC/MS for the determination of organochlorine pesticides (OCPs) in fish. In the present work, the lengthy procedures generally used in the conventional methods like, Soxhlet extraction, supercritical fluid extraction, pressurized liquid extraction and microwave assisted solvent extraction for extraction of OCPs from fish tissues are minimized by the use of two simple extraction procedures. Firstly, OCPs from fish were extracted in organic solvent with ultrasonication and then subsequently preconcentrated by single-drop micro-extraction (SDME). Extraction parameters of ultrasonication and SDME were optimized in spiked sample solution in order to obtain efficient extraction of OCPs from fish tissues. The calibration curves for OCPs were found to be linear between 10-1000 ng/g with correlation of estimations in the range 0.990-0.994. The recoveries obtained in blank fish tissues were ranged from 82.1 to 95.3%. The LOD and RSD for determination of OCPs in fish were 0.5 ng/g and 9.4-10.0%, respectively. The proposed method was applied for the determination of bioconcentration factor in fish after exposure to different concentrations of OCPs in cultured water. The present method avoids the co-extraction of lipids, long extraction steps (>12 h) and large amount of organic solvent for the separation of OCPs. The main advantages of the present method are rapid, selective, sensitive and low cost for the determination of OCPs in fish.

Lab-on-a-chip based total-phosphorus analysis device utilizing a photocatalytic reaction

NASA Astrophysics Data System (ADS)

Jung, Dong Geon; Jung, Daewoong; Kong, Seong Ho

2018-02-01

A lab-on-a-chip (LOC) device for total phosphorus (TP) analysis was fabricated for water quality monitoring. Many commercially available TP analysis systems used to estimate water quality have good sensitivity and accuracy. However, these systems also have many disadvantages such as bulky size, complex pretreatment processes, and high cost, which limit their application. In particular, conventional TP analysis systems require an indispensable pretreatment step, in which the fluidic analyte is heated to 120 °C for 30 min to release the dissolved phosphate, because many phosphates are soluble in water at a standard temperature and pressure. In addition, this pretreatment process requires elevated pressures of up to 1.1 kg cm-2 in order to prevent the evaporation of the heated analyte. Because of these limiting conditions required by the pretreatment processes used in conventional systems, it is difficult to miniaturize TP analysis systems. In this study, we employed a photocatalytic reaction in the pretreatment process. The reaction was carried out by illuminating a photocatalytic titanium dioxide (TiO2) surface formed in a microfluidic channel with ultraviolet (UV) light. This pretreatment process does not require elevated temperatures and pressures. By applying this simplified, photocatalytic-reaction-based pretreatment process to a TP analysis system, greater degrees of freedom are conferred to the design and fabrication of LOC devices for TP monitoring. The fabricated LOC device presented in this paper was characterized by measuring the TP concentration of an unknown sample, and comparing the results with those measured by a conventional TP analysis system. The TP concentrations of the unknown sample measured by the proposed LOC device and the conventional TP analysis system were 0.018 mgP/25 mL and 0.019 mgP/25 mL, respectively. The experimental results revealed that the proposed LOC device had a performance comparable to the conventional bulky TP analysis system. Therefore, our device could be directly employed in water quality monitoring as an alternative to conventional TP analysis systems.

DSS-induced acute colitis in C57BL/6 mice is mitigated by sulforaphane pre-treatment.

PubMed

Wagner, Anika E; Will, Olga; Sturm, Christine; Lipinski, Simone; Rosenstiel, Philip; Rimbach, Gerald

2013-12-01

The Brassica-derived isothiocyanate sulforaphane (SFN) is known to induce factor erythroid 2-related factor 2 (Nrf2), a transcription factor centrally involved in chemoprevention. Furthermore, SFN exhibits anti-inflammatory properties in vitro and in vivo. However, little is known regarding the anti-inflammatory properties of SFN in severe inflammatory phenotypes. In the present study, we tested if pre-treatment with SFN protects mice from dextran sodium sulphate (DSS)-induced colitis. C57BL/6 mice received either phosphate-buffered saline (control) or 25 mg/kg body weight (BW) SFN per os for 7 days. Subsequently, acute colitis was induced by administering 4% DSS via drinking water for 5 days and BWs, stool consistency and faecal blood loss were recorded. Following endoscopic colonoscopy, mice were sacrificed, the organs excised and spleen weights and colon lengths measured. For histopathological analysis, distal colon samples were fixed in 4% para-formaldehyde, sectioned and stained with hematoxylin/eosin. Inflammatory biomarkers were also measured in distal colon. Treatment with SFN prior to colitis induction significantly minimised both BW loss and the disease activity index compared to control mice. Furthermore, colon lengths in SFN pre-treated mice were significantly longer than in control mice. Both macroscopic and microscopic analysis of the colon revealed attenuated inflammation in SFN pre-treated animals. mRNA analysis of distal colon samples confirmed reduced expression of inflammatory markers and increased expression of Nrf2-dependent genes in SFN pre-treated mice. Our results indicate that pre-treating mice with SFN confers protection from DSS-induced colitis. These protective effects were corroborated macroscopically, microscopically and at the molecular level. © 2013.

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.

Surface analysis of graphite fiber reinforced polyimide composites

NASA Technical Reports Server (NTRS)

Messick, D. L.; Progar, D. J.; Wightman, J. P.

1983-01-01

Several techniques have been used to establish the effect of different surface pretreatments on graphite-polyimide composites. Composites were prepared from Celion 6000 graphite fibers and the polyimide LARC-160. Pretreatments included mechanical abrasion, chemical etching and light irradiation. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used in the analysis. Contact angle of five different liquids of varying surface tensions were measured on the composites. SEM results showed polymer-rich peaks and polymer-poor valleys conforming to the pattern of the release cloth used durng fabrication. Mechanically treated and light irradiated samples showed varying degrees of polymer peak removal, with some degradation down to the graphite fibers. Minimal changes in surface topography were observed on concentrations of surface fluorine even after pretreatment. The light irradiation pretreatment was most effective at reducing surface fluorine concentrations whereas chemical pretreatment was the least effective. Critical surface tensions correlated directly with the surface fluorine to carbon ratios as calculated from XPS.

A citrus waste-based biorefinery as a source of renewable energy: technical advances and analysis of engineering challenges.

PubMed

Rivas-Cantu, Raul C; Jones, Kim D; Mills, Patrick L

2013-04-01

An assessment of recent technical advances on pretreatment processes and its effects on enzymatic hydrolysis as the main steps of a proposed citrus processing waste (CPW) biorefinery is presented. Engineering challenges and relevant gaps in scientific and technical information for reliable design, modeling and scale up of a CPW biorefinery are also discussed. Some integrated physico-chemical pretreatments are proposed for testing for CPW, including high speed knife-grinding and simultaneous caustic addition. These new proposed processes and the effect of parameters such as particle size, surface area and morphology, pore volume and chemical composition of the diverse fractions resulting from pretreatment and enzymatic hydrolysis need to be evaluated and compared for pretreated and untreated samples of grapefruit processing waste. This assessment suggests the potential for filling the data gaps, and preliminary results demonstrate that the reduction of particle size and the increased surface area for the CPW will result in higher reaction rates and monosaccharide yields for the pretreated waste material.

Evaluation of agave bagasse recalcitrance using AFEX™, autohydrolysis, and ionic liquid pretreatments.

PubMed

Perez-Pimienta, Jose A; Flores-Gómez, Carlos A; Ruiz, Héctor A; Sathitsuksanoh, Noppadon; Balan, Venkatesh; da Costa Sousa, Leonardo; Dale, Bruce E; Singh, Seema; Simmons, Blake A

2016-07-01

A comparative analysis of the response of agave bagasse (AGB) to pretreatment by ammonia fiber expansion (AFEX™), autohydrolysis (AH) and ionic liquid (IL) was performed using 2D nuclear magnetic resonance (NMR) spectroscopy, wet chemistry, enzymatic saccharification and mass balances. It has been found that AFEX pretreatment preserved all carbohydrates in the biomass, whereas AH removed 62.4% of xylan and IL extracted 25% of lignin into wash streams. Syringyl and guaiacyl lignin ratio of untreated AGB was 4.3, whereas for the pretreated biomass the ratios were 4.2, 5.0 and 4.7 for AFEX, AH and IL, respectively. Using NMR spectra, the intensity of β-aryl ether units in aliphatic, anomeric, and aromatic regions decreased in all three pretreated samples when compared to untreated biomass. Yields of glucose plus xylose in the major hydrolysate stream were 42.5, 39.7 and 26.9kg per 100kg of untreated AGB for AFEX, IL and AH, respectively. Copyright © 2016 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.

High-performance oxygen reduction catalysts in both alkaline and acidic fuel cells based on pre-treating carbon material and iron precursor

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

Song, Ping; Barkholtz, Heather M.; Wang, Ying

We demonstrate a new and simple method for pre-treating the carbon material and iron precursor to prepare oxygen reduction reaction (ORR) catalysts, which can produce super-high performance and stability in alkaline solution, with high performance in acid solution. This strategy using cheap materials is simply controllable. Moreover, it has achieved smaller uniform nanoparticles to exhibit high stability, and the synergetic effect of Fe and N offered much higher performance in ORR than commercial Pt/C, with high maximum power density in alkaline and acid fuel cell test. So it can make this kind of catalysts be the most promising alternatives ofmore » Pt-based catalysts with best performance/price.« less

Systematization method for distinguishing plastic groups by using NIR spectroscopy.

PubMed

Kaihara, Mikio; Satoh, Minami; Satoh, Minoru

2007-07-01

A systematic classification method for polymers is not yet available in case of using near infrared spectra (NIR). That is why we have been searching for a systematic method. Because raw NIR spectra usually have few obvious peaks, NIR spectra have been pretreated by 2nd derivation for taking well modulated spectra. After the pretreatment, we applied classification and regression trees (CART) to the discrimination between the spectra and the species of polymers. As a result, we obtained a relatively simple classification tree. Judging from the obtained splitting conditions and the classified polymers, we concluded that obtained knowledge on the chemical function groups estimated by the important wavelength regions is not always applicable to this classification tree. However, we clarified the splitting rules for polymer species from the NIR spectral point of view.

Hazardous Alcohol Drinking as Predictor of Smoking Relapse (3-, 6-, and 12-Months Follow-Up) by Gender.

PubMed

Rodríguez-Cano, Rubén; López-Durán, Ana; Martínez-Vispo, Carmela; Martínez, Úrsula; Fernández Del Río, Elena; Becoña, Elisardo

2016-12-01

Diverse studies have found a relation between alcohol consumption and smoking relapse. Few studies have analyzed the relation of smoking relapse with pretreatment alcohol consumption and gender differences. The main purpose of this study is to analyze the influence of alcohol consumption in smoking relapse over 12 months (3-, 6-, and 12-months follow-up) and to determine possible gender differences. The sample included 374 smokers who quit smoking by participating in a psychological smoking cessation treatment. We assessed hazardous pretreatment alcohol drinking (AUDIT), cigarette consumption (FTND; number of cigarettes) and sociodemographic variables. Higher scores on hazardous pretreatment alcohol drinking predict smoking relapse at 3-, 6-, and 12-months after smoking cessation. In males, higher scores on hazardous pretreatment alcohol drinking predict relapse at 6 and at 12 months. In females, higher scores on hazardous pretreatment alcohol drinking predict tobacco relapse at 3 months. Hazardous pretreatment alcohol drinking predicts relapse at all intervals after smoking cessation (3-, 6-, and 12-months follow-up). However, the influence of hazardous pretreatment alcohol drinking on smoking relapse differs as a function of gender, as it is a short-term predictor in women (3 months) and a long-term predictor in men (6 and 12 months). Copyright © 2016 Elsevier Inc. All rights reserved.

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

PubMed

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

2015-09-14

To evaluate the prognostic significance of the lymphocyte to monocyte ratio (LMR) in patients with unresectable metastatic colorectal cancer who received palliative chemotherapy. 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. 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. The lymphocyte to monocyte ratio is a useful prognostic marker in patients with unresectable metastatic colorectal cancer who receive palliative chemotherapy.

Preparation of magnetic ODS-PAN thin-films for microextraction of quetiapine and clozapine in plasma and urine samples followed by HPLC-UV detection.

PubMed

Li, Dan; Zou, Juan; Cai, Pei-Shan; Xiong, Chao-Mei; Ruan, Jin-Lan

2016-06-05

In this study, conventional thin-film microextraction (TFME) was endowed with magnetic by introducing superparamagnetic SiO2@Fe3O4 nanoparticles in thin-films. Novel magnetic octadecylsilane (ODS)-polyacrylonitrile (PAN) thin-films were prepared by spraying, and used for the microextraction of quetiapine and clozapine in plasma and urine samples, followed by the detection of HPLC-UV. The influencing factors on the extraction efficiency of magnetic ODS-PAN TFME, including pH, extraction time, desorption solvent, desorption time, and ion strength were investigated systematically. Under the optimal conditions, both analytes showed good linearity over ranges of 0.070-9.000μgmL(-1) and 0.012-9.000μgmL(-1) in plasma and urine samples, respectively, with correlation coefficients (R(2)) above 0.9990. Limits of detection (LODs) for quetiapine in plasma and urine samples were 0.013 and 0.003μgmL(-1), respectively. LODs for clozapine in plasma and urine samples were 0.015 and 0.003μgmL(-1), respectively. The relative standard deviations (RSDs) for quetiapine and clozapine were less than 9.23%. After the validation, the protocol was successfully applied for the determination of quetiapine and clozapine in patients' plasma and urine samples with satisfactory recoveries between 99-110%. The proposed magnetic ODS-PAN TFME was very simple, fast and easy to handle. It showed high potential as a powerful pretreatment technology for routine therapeutic drug monitoring (TDM) in plasma and urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and validation of amitriptyline and its metabolite in human plasma by ultra performance liquid chromatography-tandem mass spectrometry and its application to a bioequivalence study.

PubMed

Bhatt, Mitesh; Shah, Sanjay

2010-11-01

A method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in combination with solid-phase extraction for sample pretreatment has been developed for the simultaneous analysis of amitriptyline and its main metabolite in human plasma. The extraction of the analytes from plasma samples was carried out by means of a selective SPE procedure using hydrophilic-lipophilic balance cartridges. The assay involves a simple solid-phase extraction (SPE) procedure of 0.2 mL of human plasma and analysis was performed on a triple-quadrupole tandem mass spectrometer by multiple reactions monitoring (MRM) mode via electrospray ionization (ESI). The standard calibration curve was linear over the ranges 0.370-95.539 ng/mL for amitriptyline and 0.365-94.374 ng/mL for nortriptyline, expressed by the linear correlation coefficient r², which was better than 0.995 for both. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recovery was 85.3, 88.4 and 80.7% for amitriptyline, nortriptyline and doxepin respectively. Total run time was 1.2 min only for each sample, which makes it possible to analyze more than 400 samples per day. The method was highly reproducible and gave peaks with excellent chromatography properties. Copyright © 2010 John Wiley & Sons, Ltd.

Optimization of a new method for extraction of cyanidin chloride and pelargonidin chloride anthocyanins with magnetic solid phase extraction and determination in fruit samples by HPLC with central composite design.

PubMed

Yari, Abdollah; Rashnoo, Saba

2017-11-01

Here, we are reporting a sensitive, simple and rapid method for the analysis of cyanidin chloride and pelargonidin chloride anthocyanins in cherry, sour cherry, pomegranate and barberry produced in Iran. The analytes were extracted with acetonitrile-hydrochloric acid (1% v/v) mixture under optimized pretreatment conditions. Clean-up of the extract from fruits was conducted by magnetic solid phase extraction using salicylic acid functionalized silica-coated magnetite nanoparticles (SCMNPs) as the adsorbent. The optimized conditions searched with central composite design. Working under optimum conditions specified as: SCMNPs modified with salicylic acid, sorbent contact time and sample 10min, mechanical stirring time 57.3min. HPLC with UV-detection was used for determination of the analytes. The limit of detection, LOD, obtained for the two anthocyanins were 0.02 and 0.03μgg -1 , respectively. The ranges of the spiked recoveries were 80.0-97.6 and 72.9-97.2%, with the relative standard deviations (RSD) of 2.1 and 2.5%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of antimony microparticles supported on biochar for application in the voltammetric determination of paraquat.

PubMed

Gevaerd, Ava; de Oliveira, Paulo R; Mangrich, Antonio S; Bergamini, Márcio F; Marcolino-Junior, Luiz H

2016-05-01

This work describes the construction and application of carbon paste electrodes modified with biochar and antimony microparticles (SbBCPE) for voltammetric determination of paraquat using a simple and sensitive procedure based on voltammetric stripping analysis. Some parameters such as amount of biochar and antimony used in the composition of the carbon paste and instrumental parameters were examined in detail. Under optimized conditions, an analytical curve was obtained for paraquat determination employing SbBCPE, which showed a linear response ranging from 0.2 to 2.9 μmol L(-1), with limit of detection and quantification of 34 nmol L(-1) and 113 nmol L(-1), respectively, after paraquat pre-concentration of 120 s. The repeatability study presented a RSD=2.0% for 10 consecutive measurements using the same electrode surface and the reproducibility study showed a RSD=2.7% for measurements with 10 different electrode surfaces. The proposed sensor was successfully applied for paraquat determination in tap water and citric fruit juice spiked samples and good recoveries were obtained without any sample pre-treatment, showing its promising analytical performance. Copyright © 2016 Elsevier B.V. All rights reserved.

[Rapid determination of illicit beta2-agonist additives in health foods and traditional Chinese patent medicines with DCBI-MS/MS method].

PubMed

Hou, Yu-Lan; Wu, Shuang; Wang, Hua; Zhao, Yong; Liao, Peng; Tian, Qing-Qing; Sun, Wen-Jian; Chen, Bo

2013-01-01

A novel rapid method for detection of the illicit beta2-agonist additives in health foods and traditional Chinese patent medicines was developed with the desorption corona beam ionization mass spectrometry (DCBI-MS) technique. The DCBI conditions including temperature and sample volume were optimized according to the resulting mass spectra intensity. Matrix effect on 9 beta2-agonists additives was not significant in the proposed rapid determination procedure. All of the 9 target molecules were detected within 1 min. Quantification was achieved based on the typical fragment ion in MS2 spectra of each analyte. The method showed good linear coefficients in the range of 1-100 mg x L(-1) for all analytes. The relative deviation values were between 14.29% and 25.13%. Ten claimed antitussive and antiasthmatic health foods and traditional Chinese patent medicines from local pharmacies were analyzed. All of them were negative with the proposed DCBI-MS method. Without tedious sample pretreatments, the developed DCBI-MS is simple, rapid and sensitive for rapid qualification and semi-quantification of the illicit beta2-agonist additives in health foods and traditional Chinese patent medicines.

Glass transition in thin supported polystyrene films probed by temperature-modulated ellipsometry in vacuum.

PubMed

Efremov, Mikhail Yu; Kiyanova, Anna V; Last, Julie; Soofi, Shauheen S; Thode, Christopher; Nealey, Paul F

2012-08-01

Glass transition in thin (1-200 nm thick) spin-cast polystyrene films on silicon surfaces is probed by ellipsometry in a controlled vacuum environment. A temperature-modulated modification of the method is used alongside a traditional linear temperature scan. A clear glass transition is detected in films with thicknesses as low as 1-2 nm. The glass transition temperature (T(g)) shows no substantial dependence on thickness for coatings greater than 20 nm. Thinner films demonstrate moderate T(g) depression achieving 18 K for thicknesses 4-7 nm. Less than 4 nm thick samples are excluded from the T(g) comparison due to significant thickness nonuniformity (surface roughness). The transition in 10-20 nm thick films demonstrates excessive broadening. For some samples, the broadened transition is clearly resolved into two separate transitions. The thickness dependence of the glass transition can be well described by a simple 2-layer model. It is also shown that T(g) depression in 5 nm thick films is not sensitive to a wide range of experimental factors including molecular weight characteristics of the polymer, specifications of solvent used for spin casting, substrate composition, and pretreatment of the substrate surface.

Chiral metabonomics: 1H NMR-based enantiospecific differentiation of metabolites in human urine via direct cosolvation with β-cyclodextrin.

PubMed

Pérez-Trujillo, Míriam; Lindon, John C; Parella, Teodor; Keun, Hector C; Nicholson, Jeremy K; Athersuch, Toby J

2012-03-20

Differences in molecular chirality remain an important issue in drug metabolism and pharmacokinetics for the pharmaceutical industry and regulatory authorities, and chirality is an important feature of many endogenous metabolites. We present a method for the rapid, direct differentiation and identification of chiral drug enantiomers in human urine without pretreatment of any kind. Using the well-known anti-inflammatory chemical ibuprofen as one example, we demonstrate that the enantiomers of ibuprofen and the diastereoisomers of one of its main metabolites, the glucuronidated carboxylate derivative, can be resolved by (1)H NMR spectroscopy as a consequence of direct addition of the chiral cosolvating agent (CSA) β-cyclodextrin (βCD). This approach is simple, rapid, and robust, involves minimal sample manipulation, and does not require derivatization or purification of the sample. In addition, the method should allow the enantiodifferentiation of endogenous chiral metabolites, and this has potential value for differentiating metabolites from mammalian and microbial sources in biofluids. From these initial findings, we propose that more extensive and detailed enantiospecific metabolic profiling could be possible using CSA-NMR spectroscopy than has been previously reported.

Rapid detection of Salmonella in milk by electrochemical magneto-immunosensing.

PubMed

Liébana, Susana; Lermo, Anabel; Campoy, Susana; Cortés, María Pilar; Alegret, Salvador; Pividori, María Isabel

2009-10-15

A very simple and rapid method for the detection of Salmonella in milk is reported. In this approach, the bacteria are captured and preconcentrated from milk samples with magnetic beads through an immunological reaction. A second polyclonal antibody labeled with peroxidase is used as serological confirmation with electrochemical detection based on a magneto-electrode. The 'IMS/m-GEC electrochemical immunosensing' approach shows a limit of detection of 5 x 10(3) and 7.5 x 10(3)CFU mL(-1) in LB and in milk diluted 1/10 in LB broth, respectively, in 50 min without any pretreatment. If the skimmed-milk is preenriched for 6h, the method is able to detect as low as 1.4 CFU mL(-1), while if it is preenriched for 8h, as low as 0.108 x CFU mL(-1) (2.7 x CFU in 25 g of milk, in 5 samples of 5 mL) are detected accordingly with the legislation. Moreover, the method is able to clearly distinguish between food pathogenic bacteria such as Salmonella and Escherichia coli. The features of this approach are discussed and compared with classical culture methods.

Impact of Thermal Pretreatment Temperatures on Woody Biomass Chemical Composition, Physical Properties and Microstructure

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

Wang, Ping; Howard, Bret H.

Thermal pretreatment of biomass by torrefaction and low temperature pyrolysis has the potential for generating high quality and more suitable fuels. To utilize a model to describe the complex and dynamic changes taking place during these two treatments for process design, optimization and scale-up, detailed data is needed on the property evolution during treatment of well-defined individual biomass particles. The objectives of this study are to investigate the influence of thermal pretreatment temperatures on wood biomass biochemical compositions, physical properties and microstructure. Wild cherry wood was selected as a model biomass and prepared for this study. The well-defined wood particlemore » samples were consecutively heated at 220, 260, 300, 350, 450 and 550 °C for 0.5 h under nitrogen. Untreated and treated samples were characterized for biochemical composition changes (cellulose, hemicellulose, and lignin) by thermogravimetric analyzer (TGA), physical properties (color, dimensions, weight, density and grindablity), chemical property (proximate analysis and heating value) and microstructural changes by scanning electron microscopy (SEM). Hemicellulose was mostly decomposed in the samples treated at 260 and 300 °C and resulted in the cell walls weakening resulting in improved grindability. The dimensions of the wood were reduced in all directions and shrinkage increased with increased treatment temperature and weight loss. With increased treatment temperature, losses of weight and volume increased and bulk density decreased. The low temperature pyrolyzed wood samples improved solid fuel property with high fuel ratio, which are close to lignite/bituminous coal. Morphology of the wood remained intact through the treatment range but the cell walls were thinner. Lastly, these results will improve the understanding of the property changes of the biomass during pretreatment and will help to develop models for process simulation and potential application of the treated biomass.« less

Impact of Thermal Pretreatment Temperatures on Woody Biomass Chemical Composition, Physical Properties and Microstructure

DOE PAGES

Wang, Ping; Howard, Bret H.

2017-12-23

Thermal pretreatment of biomass by torrefaction and low temperature pyrolysis has the potential for generating high quality and more suitable fuels. To utilize a model to describe the complex and dynamic changes taking place during these two treatments for process design, optimization and scale-up, detailed data is needed on the property evolution during treatment of well-defined individual biomass particles. The objectives of this study are to investigate the influence of thermal pretreatment temperatures on wood biomass biochemical compositions, physical properties and microstructure. Wild cherry wood was selected as a model biomass and prepared for this study. The well-defined wood particlemore » samples were consecutively heated at 220, 260, 300, 350, 450 and 550 °C for 0.5 h under nitrogen. Untreated and treated samples were characterized for biochemical composition changes (cellulose, hemicellulose, and lignin) by thermogravimetric analyzer (TGA), physical properties (color, dimensions, weight, density and grindablity), chemical property (proximate analysis and heating value) and microstructural changes by scanning electron microscopy (SEM). Hemicellulose was mostly decomposed in the samples treated at 260 and 300 °C and resulted in the cell walls weakening resulting in improved grindability. The dimensions of the wood were reduced in all directions and shrinkage increased with increased treatment temperature and weight loss. With increased treatment temperature, losses of weight and volume increased and bulk density decreased. The low temperature pyrolyzed wood samples improved solid fuel property with high fuel ratio, which are close to lignite/bituminous coal. Morphology of the wood remained intact through the treatment range but the cell walls were thinner. Lastly, these results will improve the understanding of the property changes of the biomass during pretreatment and will help to develop models for process simulation and potential application of the treated biomass.« less

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.

Optimization of Alkaline and Dilute Acid Pretreatment of Agave Bagasse by Response Surface Methodology.

PubMed

Ávila-Lara, Abimael I; Camberos-Flores, Jesus N; Mendoza-Pérez, Jorge A; Messina-Fernández, Sarah R; Saldaña-Duran, Claudia E; Jimenez-Ruiz, Edgar I; Sánchez-Herrera, Leticia M; Pérez-Pimienta, Jose A

2015-01-01

Utilization of lignocellulosic materials for the production of value-added chemicals or biofuels generally requires a pretreatment process to overcome the recalcitrance of the plant biomass for further enzymatic hydrolysis and fermentation stages. Two of the most employed pretreatment processes are the ones that used dilute acid (DA) and alkaline (AL) catalyst providing specific effects on the physicochemical structure of the biomass, such as high xylan and lignin removal for DA and AL, respectively. Another important effect that need to be studied is the use of a high solids pretreatment (≥15%) since offers many advantaged over lower solids loadings, including increased sugar and ethanol concentrations (in combination with a high solids saccharification), which will be reflected in lower capital costs; however, this data is currently limited. In this study, several variables, such as catalyst loading, retention time, and solids loading, were studied using response surface methodology (RSM) based on a factorial central composite design of DA and AL pretreatment on agave bagasse using a range of solids from 3 to 30% (w/w) to obtain optimal process conditions for each pretreatment. Subsequently enzymatic hydrolysis was performed using Novozymes Cellic CTec2 and HTec2 presented as total reducing sugar (TRS) yield. Pretreated biomass was characterized by wet-chemistry techniques and selected samples were analyzed by calorimetric techniques, and scanning electron/confocal fluorescent microscopy. RSM was also used to optimize the pretreatment conditions for maximum TRS yield. The optimum conditions were determined for AL pretreatment: 1.87% NaOH concentration, 50.3 min and 13.1% solids loading, whereas DA pretreatment: 2.1% acid concentration, 33.8 min and 8.5% solids loading.

Optimization of Alkaline and Dilute Acid Pretreatment of Agave Bagasse by Response Surface Methodology

PubMed Central

Ávila-Lara, Abimael I.; Camberos-Flores, Jesus N.; Mendoza-Pérez, Jorge A.; Messina-Fernández, Sarah R.; Saldaña-Duran, Claudia E.; Jimenez-Ruiz, Edgar I.; Sánchez-Herrera, Leticia M.; Pérez-Pimienta, Jose A.

2015-01-01

Utilization of lignocellulosic materials for the production of value-added chemicals or biofuels generally requires a pretreatment process to overcome the recalcitrance of the plant biomass for further enzymatic hydrolysis and fermentation stages. Two of the most employed pretreatment processes are the ones that used dilute acid (DA) and alkaline (AL) catalyst providing specific effects on the physicochemical structure of the biomass, such as high xylan and lignin removal for DA and AL, respectively. Another important effect that need to be studied is the use of a high solids pretreatment (≥15%) since offers many advantaged over lower solids loadings, including increased sugar and ethanol concentrations (in combination with a high solids saccharification), which will be reflected in lower capital costs; however, this data is currently limited. In this study, several variables, such as catalyst loading, retention time, and solids loading, were studied using response surface methodology (RSM) based on a factorial central composite design of DA and AL pretreatment on agave bagasse using a range of solids from 3 to 30% (w/w) to obtain optimal process conditions for each pretreatment. Subsequently enzymatic hydrolysis was performed using Novozymes Cellic CTec2 and HTec2 presented as total reducing sugar (TRS) yield. Pretreated biomass was characterized by wet-chemistry techniques and selected samples were analyzed by calorimetric techniques, and scanning electron/confocal fluorescent microscopy. RSM was also used to optimize the pretreatment conditions for maximum TRS yield. The optimum conditions were determined for AL pretreatment: 1.87% NaOH concentration, 50.3 min and 13.1% solids loading, whereas DA pretreatment: 2.1% acid concentration, 33.8 min and 8.5% solids loading. PMID:26442260

Ultrasound pretreatment for enhanced biogas production from olive mill wastewater.

PubMed

Oz, Nilgun Ayman; Uzun, Alev Cagla

2015-01-01

This study investigates applicability of low frequency ultrasound technology to olive mill wastewaters (OMWs) as a pretreatment step prior to anaerobic batch reactors to improve biogas production and methane yield. OMWs originating from three phase processes are characterized with high organic content and complex nature. The treatment of the wastewater is problematic and alternative treatment options should be investigated. In the first part of the study, OMW samples were subjected to ultrasound at a frequency of 20kHz with applied powers varying between 50 and 100W under temperature controlled conditions for different time periods in order to determine the most effective sonication conditions. The level of organic matter solubilization at ultrasound experiments was assessed by calculating the ratio of soluble chemical oxygen demand/total chemical oxygen demand (SCOD/TCOD). The results revealed that the optimum ultrasonic condition for diluted OMW is 20kHz, 0.4W/mL for 10min. The application of ultrasound to OMW increased SCOD/TCOD ratio from 0.59 to 0.79. Statistical analysis (Friedman's tests) show that ultrasound was significantly effective on diluted OMW (p<0.05) in terms of SCOD parameter, but not for raw OMW (p>0.05). For raw OMW, this increase has been found to be limited due to high concentration of suspended solids (SS). In the second part of the study, biogas and methane production rates of anaerobic batch reactor fed with the ultrasound pretreated OMW samples were compared with the results of control reactor fed with untreated OMW in order to determine the effect of sonication. A nonparametric statistical procedure, Mann-Whitney U test, was used to compare biogas and methane production from anaerobic batch reactors for control and ultrasound pretreated samples. Results showed that application of low frequency ultrasound to OMW significantly improved both biogas and methane production in anaerobic batch reactor fed with the wastewater (p<0.05). Anaerobic batch reactor fed with ultrasound pretreated diluted OMW produced approximately 20% more biogas and methane compared with the untreated one (control reactor). The overall results indicated that low frequency ultrasound pretreatment increased soluble COD in OMW and subsequently biogas production. Copyright © 2014 Elsevier B.V. All rights reserved.

Glycerol carbonate as green solvent for pretreatment of sugarcane bagasse

PubMed Central

2013-01-01

Background Pretreatment of lignocellulosic biomass is a prerequisite for effective saccharification to produce fermentable sugars. In this study, “green” solvent systems based on acidified mixtures of glycerol carbonate (GC) and glycerol were used to treat sugarcane bagasse and the roles of each solvent in deconstructing biomass were determined. Results Pretreatment of sugarcane bagasse at 90°C for only 30 min with acidified GC produced a solid residue having a glucan digestibility of 90% and a glucose yield of 80%, which were significantly higher than a glucan digestibility of 16% and a glucose yield of 15% obtained for bagasse pretreated with acidified ethylene carbonate (EC). Biomass compositional analyses showed that GC pretreatment removed more lignin than EC pretreatment (84% vs 54%). Scanning electron microscopy (SEM) showed that fluffy and size-reduced fibres were produced from GC pretreatment whereas EC pretreatment produced compact particles of reduced size. The maximal glucan digestibility and glucose yield of GC/glycerol systems were about 7% lower than those of EC/ethylene glycol (EG) systems. Replacing up to 50 wt% of GC with glycerol did not negatively affect glucan digestibility and glucose yield. The results from pretreatment of microcrystalline cellulose (MCC) showed that (1) pretreatment with acidified alkylene glycol (AG) alone increased enzymatic digestibility compared to pretreatments with acidified alkylene carbonate (AC) alone and acidified mixtures of AC and AG, (2) pretreatment with acidified GC alone slightly increased, but with acidified EC alone significantly decreased, enzymatic digestibility compared to untreated MCC, and (3) there was a good positive linear correlation of enzymatic digestibility of treated and untreated MCC samples with congo red (CR) adsorption capacity. Conclusions Acidified GC alone was a more effective solvent for pretreatment of sugarcane bagasse than acidified EC alone. The higher glucose yield obtained with GC-pretreated bagasse is possibly due to the presence of one hydroxyl group in the GC molecular structure, resulting in more significant biomass delignification and defibrillation, though both solvent pretreatments reduced bagasse particles to a similar extent. The maximum glucan digestibility of GC/glycerol systems was less than that of EC/EG systems, which is likely attributed to glycerol being less effective than EG in biomass delignification and defibrillation. Acidified AC/AG solvent systems were more effective for pretreatment of lignin-containing biomass than MCC. PMID:24156757

Multicentre validation of IMRT pre-treatment verification: comparison of in-house and external audit.

PubMed

Jornet, Núria; Carrasco, Pablo; Beltrán, Mercè; Calvo, Juan Francisco; Escudé, Lluís; Hernández, Victor; Quera, Jaume; Sáez, Jordi

2014-09-01

We performed a multicentre intercomparison of IMRT optimisation and dose planning and IMRT pre-treatment verification methods and results. The aims were to check consistency between dose plans and to validate whether in-house pre-treatment verification results agreed with those of an external audit. Participating centres used two mock cases (prostate and head and neck) for the intercomparison and audit. Compliance to dosimetric goals and total number of MU per plan were collected. A simple quality index to compare the different plans was proposed. We compared gamma index pass rates using the centre's equipment and methodology to those of an external audit. While for the prostate case, all centres fulfilled the dosimetric goals and plan quality was homogeneous, that was not the case for the head and neck case. The number of MU did not correlate with the plan quality index. Pre-treatment verifications results of the external audit did not agree with those of the in-house measurements for two centres: being within tolerance for in-house measurements and unacceptable for the audit or the other way round. Although all plans fulfilled dosimetric constraints, plan quality is highly dependent on the planner expertise. External audits are an excellent tool to detect errors in IMRT implementation and cannot be replaced by intercomparison using results obtained by centres. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Ultrasound assisted biogas production from co-digestion of wastewater sludges and agricultural wastes: Comparison with microwave pre-treatment.

PubMed

Aylin Alagöz, B; Yenigün, Orhan; Erdinçler, Ayşen

2018-01-01

This study investigates the effect of ultrasonication and microwave sludge disintegration/pre-treatment techniques on the anaerobic co-digestion efficiency of wastewater sludges with olive and grape pomaces. The effects of both co-digestion and sludge pre-treatment techniques were evaluated in terms of the organic removal efficiency and the biogas production. The "co-digestion" of wastewater sludge with both types of pomaces was revealed to be a much more efficient way for the biogas production compared to the single (mono) sludge digestion. The ultrasonication and microwave pre-treatments applied to the sludge samples caused to a further increase in biogas and methane yields. Based on applied specific energies, ultrasonication pre-treatment was found much more effective than microwave irradiation. The specific energy applied in microwave pre-treatment (87,000kj/kgTS) was almost 9 times higher than that of used in ultrasonication (10,000kj/kgTS), resulting only 10-15% increases in biogas/methane yield. Co-digestion of winery and olive industry residues with pre-treated wastewater sludges appears to be a suitable technique for waste management and energy production. Copyright © 2017 Elsevier B.V. All rights reserved.

A green and efficient technology for the degradation of cellulosic materials: structure changes and enhanced enzymatic hydrolysis of natural cellulose pretreated by synergistic interaction of mechanical activation and metal salt.

PubMed

Zhang, Yanjuan; Li, Qian; Su, Jianmei; Lin, Ye; Huang, Zuqiang; Lu, Yinghua; Sun, Guosong; Yang, Mei; Huang, Aimin; Hu, Huayu; Zhu, Yuanqin

2015-02-01

A new technology for the pretreatment of natural cellulose was developed, which combined mechanical activation (MA) and metal salt treatments in a stirring ball mill. Different valent metal nitrates were used to investigate the changes in degree of polymerization (DP) and crystallinity index (CrI) of cellulose after MA+metal salt (MAMS) pretreatment, and Al(NO3)3 showed better pretreatment effect than NaNO3 and Zn(NO3)2. The destruction of morphological structure of cellulose was mainly resulted from intense ball milling, and the comparative studies on the changes of DP and crystal structure of MA and MA+Al(NO3)3 pretreated cellulose samples showed a synergistic interaction of MA and Al(NO3)3 treatments with more effective changes of structural characteristics of MA+Al(NO3)3 pretreated cellulose and substantial increase of reducing sugar yield in enzymatic hydrolysis of cellulose. In addition, the results indicated that the presence of Al(NO3)3 had significant enhancement for the enzymatic hydrolysis of cellulose. Copyright © 2014 Elsevier Ltd. All rights reserved.

Enhancement of anaerobic digestion efficiency of wastewater sludge and olive waste: Synergistic effect of co-digestion and ultrasonic/microwave sludge pre-treatment.

PubMed

Alagöz, B Aylin; Yenigün, Orhan; Erdinçler, Ayşen

2015-12-01

This study investigates the effect of ultrasonic and microwave pre-treatment on biogas production from the anaerobic co-digestion of olive pomace and wastewater sludges. It was found that co-digestion of wastewater sludge with olive pomace yielded around 0.21 L CH4/g VS added, whereas the maximum methane yields from the mono-digestion of olive pomace and un-pretreated wastewater sludges were 0.18 and 0.16L CH4/g VS added. In the same way, compared to mono-digestion of these substrates, co-digestion increased methane production by 17-31%. The microwave and ultrasonic pre-treatments applied to sludge samples prior to co-digestion process led to further increase in the methane production by 52% and 24%, respectively, compared to co-digestion with un-pretreated wastewater sludge. The highest biogas and methane yields were obtained from the co-digestion of 30 min microwave pre-treated wastewater sludges and olive pomace to be 0.46 L/g VS added and 0.32 L CH4/g VS added, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of anatomical fractionation on the enzymatic hydrolysis of acid and alkaline pretreated corn stover.

PubMed

Duguid, K B; Montross, M D; Radtke, C W; Crofcheck, C L; Wendt, L M; Shearer, S A

2009-11-01

Due to concerns with biomass collection systems and soil sustainability there are opportunities to investigate the optimal plant fractions to collect for conversion. An ideal feedstock would require a low severity pretreatment to release a maximum amount of sugar during enzymatic hydrolysis. Corn stover fractions were separated manually and analyzed for glucan, xylan, acid soluble lignin, acid insoluble lignin, and ash composition. The stover fractions were also pretreated with either 0%, 0.4%, or 0.8% NaOH for 2 h at room temperature, washed, autoclaved and saccharified. In addition, dilute sulfuric acid pretreated samples underwent simultaneous saccharification and fermentation (SSF) to ethanol. In general, the two pretreatments produced similar trends with cobs, husks, and leaves responding best to the pretreatments, the tops of stalks responding slightly less, and the bottom of the stalks responding the least. For example, corn husks pretreated with 0.8% NaOH released over 90% (standard error of 3.8%) of the available glucan, while only 45% (standard error of 1.1%) of the glucan was produced from identically treated stalk bottoms. Estimates of the theoretical ethanol yield using acid pretreatment followed by SSF were 65% (standard error of 15.9%) for husks and 29% (standard error of 1.8%) for stalk bottoms. This suggests that integration of biomass collection systems to remove sustainable feedstocks could be integrated with the processes within a biorefinery to minimize overall ethanol production costs.

Optimizing on-farm pretreatment of perennial grasses for fuel ethanol production.

PubMed

Digman, Matthew F; Shinners, Kevin J; Casler, Michael D; Dien, Bruce S; Hatfield, Ronald D; Jung, Hans-Joachim G; Muck, Richard E; Weimer, Paul J

2010-07-01

Switchgrass (Panicum virgatum L.) and reed canarygrass (Phalaris arundinacea L.) were pretreated under ambient temperature and pressure with sulfuric acid and calcium hydroxide in separate experiments. Chemical loadings from 0 to 100g (kg DM)(-1) and durations of anaerobic storage from 0 to 180days were investigated by way of a central composite design at two moisture contents (40% or 60% w.b.). Pretreated and untreated samples were fermented to ethanol by Saccharomyces cerevisiae D5A in the presence of a commercially available cellulase (Celluclast 1.5L) and beta-glucosidase (Novozyme 188). Xylose levels were also measured following fermentation because xylose is not metabolized by S. cerevisiae. After sulfuric acid pretreatment and anaerobic storage, conversion of cell wall glucose to ethanol for reed canarygrass ranged from 22% to 83% whereas switchgrass conversions ranged from 16% to 46%. Pretreatment duration had a positive effect on conversion but was mitigated with increased chemical loadings. Conversions after calcium hydroxide pretreatment and anaerobic storage ranged from 21% to 55% and 18% to 54% for reed canarygrass and switchgrass, respectively. The efficacy of lime pretreatment was found to be highly dependent on moisture content. Moreover, pretreatment duration was only found to be significant for reed canarygrass. Although significant levels of acetate and lactate were observed in the biomass after storage, S. cerevisiae was not found to be inhibited at a 10% solids loading. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

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.

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

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

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.

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

Determination of the acute toxicities of physicochemical pretreatment and advanced oxidation processes applied to dairy effluents on activated sludge.

PubMed

Sivrioğlu, Özge; Yonar, Taner

2015-04-01

In this study, the acute toxicities of raw, physicochemical pre-treated, ozonated, and Fenton reagent applied samples of dairy wastewater toward activated sludge microorganisms, evaluated using the International Organization for Standardization's respiration inhibition test (ISO 8192), are presented. Five-day biological oxygen demand (BOD5) was measured to determine the biodegradability of physicochemical treatment, ozonation, Fenton oxidation or no treatment (raw samples) of dairy wastewater. Chemical pretreatment positively affected biodegradability, and the inhibition exhibited by activated sludge was removed to a considerable degree. Ozonation and the Fenton process exhibited good chemical oxygen demand removal (61%) and removal of toxins. Low sludge production was observed for the Fenton process applied to dairy effluents. We did not determine the inhibitory effect of the Fenton-process on the activated sludge mixture. The pollutant-removal efficiencies of the applied processes and their associated operating costs were determined. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Tea Polyphenol-Reduced Graphene Oxide Deposition on Titanium Surface Enhances Osteoblast Bioactivity.

PubMed

Liu, Mengting; Hao, Liying; Huang, Qian; Zhao, Dan; Li, Qianshun; Cai, Xiaoxiao

2018-05-01

Graphene, a novel carbon-based material, has been widely used as osteogenic agent for the potential effect on the promotion of osteoblast proliferation. Tea polyphenol-reduced graphene oxide (TPG) is a simple and environmental-friendly raw material to obtain graphene. In this study, TPG was deposited on the Ti substrate to promote the bone regeneration. We prepared a honeycomb-like structure by acid and alkali pretreatment and immobilized the TPG layer (Ti-TPG) on the surface via electrochemical deposition. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD) were used to identify the immobilization of TPG on the titanium (Ti) successfully. Furthermore, the biological response of the Ti-TPG surface to rat osteoblast was evaluated. We also studied the cell adhesion, proliferation and expression of ossification genes on the sample. The results revealed that Ti-TPG had an advantage over Ti alloys in modulating cellular activity and Ti-TPG may be a promising coating for biological materials.

New approach to the determination of contaminants of emerging concern in natural water: study of alprazolam employing adsorptive cathodic stripping voltammetry.

PubMed

Nunes, Chalder Nogueira; Pauluk, Lucas Ely; Dos Anjos, Vanessa Egéa; Lopes, Mauro Chierici; Quináia, Sueli Pércio

2015-08-01

Contaminants of emerging concern (CECs) are chemicals, including pharmaceutical and personal care products, not commonly monitored in the aquatic environment. Pharmaceuticals are nowadays considered as an important environmental contaminant. Chromatography methods which require expensive equipment and complicated sample pretreatment are used for detection of CECs in natural water. Thus, in this study we proposed a simple, fast, and low-cost voltammetric method as a screening tool for the determination of CECs in natural water prior to chromatography. A case study was conducted with alprazolam (benzodiazepine). The method was optimized and validated in-house. The limit of quantification was 0.4 μg L(-1) for a 120 s preconcentration time. The recoveries ranged from 93 to 120 % for accuracy tests. A further proposal aim was to determine for the first time the occurrence of alprazolam in Brazilian river water and to evaluate its potential use as a marker of contamination by wastewater.

A new technique for spectrophotometric determination of pseudoephedrine and guaifenesin in syrup and synthetic mixture.

PubMed

Riahi, Siavash; Hadiloo, Farshad; Milani, Seyed Mohammad R; Davarkhah, Nazila; Ganjali, Mohammad R; Norouzi, Parviz; Seyfi, Payam

2011-05-01

The accuracy in predicting different chemometric methods was compared when applied on ordinary UV spectra and first order derivative spectra. Principal component regression (PCR) and partial least squares with one dependent variable (PLS1) and two dependent variables (PLS2) were applied on spectral data of pharmaceutical formula containing pseudoephedrine (PDP) and guaifenesin (GFN). The ability to derivative in resolved overlapping spectra chloropheniramine maleate was evaluated when multivariate methods are adopted for analysis of two component mixtures without using any chemical pretreatment. The chemometrics models were tested on an external validation dataset and finally applied to the analysis of pharmaceuticals. Significant advantages were found in analysis of the real samples when the calibration models from derivative spectra were used. It should also be mentioned that the proposed method is a simple and rapid way requiring no preliminary separation steps and can be used easily for the analysis of these compounds, especially in quality control laboratories. Copyright © 2011 John Wiley & Sons, Ltd.

Detection of enteropathogenic Escherichia coli by microchip capillary electrophoresis.

PubMed

Law, Wai S; Li, Sam F Y; Kricka, Larry J

2009-01-01

There is always a need to detect the presence of microorganisms, either as contaminants in food and pharmaceutical industries or bioindicators for disease diagnosis. Hence, it is important to develop efficient, rapid, and simple methods to detect microorganisms. Traditional culturing method is unsatisfactory due to its long incubation time. Molecular methods, although capable of providing a high degree of specificity, are not always useful in providing quick tests of presence or absence of microorganisms. Microchip elec-trophoresis has been recently employed to address problems associated with the detection of microorganisms due to its high versatility, selectivity, sensitivity, and short analysis times. In this work, the potential of PDMS-based microchip electrophoresis in the identification and characterization of microorganism was evaluated. Enteropathogenic E. coli (EPEC) was selected as the model microorganism. To obtain repeat-able separations, sample pretreatment was found to be essential. Microchip electrophoresis with laser-induced fluorescence detection could potentially revolutionize certain aspects of microbiology involving diagnosis, profiling of pathogens, environmental analysis, and many others areas of study.

Analysis of hop-derived terpenoids in beer and evaluation of their behavior using the stir bar-sorptive extraction method with GC-MS.

PubMed

Kishimoto, Toru; Wanikawa, Akira; Kagami, Noboru; Kawatsura, Katsuyuki

2005-06-15

Hop aroma components, which mainly comprise terpenoids, contribute to the character of beers. However, pretreatments are necessary before analyzing these components because of their trace levels and complicated matrixes. Here, the stir bar-sorptive extraction (SBSE) method was used to detect and quantify many terpenoids simultaneously from small samples. This simple technique showed low coefficients of variation, high accuracy, and low detection limits. An investigation of the behavior of terpenoids identified two distinct patterns of decreasing concentration during wort boiling. The first, which was seen in myrcene and linalool, involved a rapid decrease that was best fitted by a quadratic curve. The second, which was observed in beta-eudesmol, humulene, humulene epoxide I, beta-farnesene, caryophyllene, and geraniol, involved a gentle linear decrease. Conversely, the concentration of beta-damascenone increased after boiling. As the aroma composition depended on the hop variety, we also examined the relationship between terpenoid content and sensory analysis in beer.

Determination of multiresidues of three acid herbicides in tobacco by liquid chromatography/tandem mass spectrometry.

PubMed

Liu, Shanshan; Bian, Zhaoyang; Yang, Fei; Li, Zhonghao; Fan, Ziyan; Zhang, Hongfei; Wang, Ying; Zhang, Yange; Tang, Gangling

2015-01-01

A method to determine residues of the three acid herbicides, 2,4,5-trichlorophenoxyacetic acid, 2,4-dichlorophenoxyacetic acid, and 3,6-dichloro-2-methoxybenzoic acid (dicamba), in tobacco using LC/MS/MS is presented. Because these herbicide residues in tobacco might exist in different forms (free acid, salt, and ester), tobacco samples were first pretreated by alkaline hydrolysis and then the pH was adjusted in order to convert the residues completely to their free acid forms. Dichloromethane extraction and dispersive SPE using C18 sorbent were carried out before LC/MS/MS analysis, and quantification was performed using the internal standard method. Linearity was good for all analytes (R(2) ≥ 0.999) in the concentration range of 0.02 to 0.5 mg/kg. LODs were below 0.05 mg/kg. Recoveries ranged from 80.4 to 93.5%, and RSD was below 10%. This simple, efficient, and sensitive method can be applied to the determination of residues of the three acid herbicides in tobacco.

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.

Effect of ultrasound treatment on the water state in kiwifruit during osmotic dehydration.

PubMed

Nowacka, M; Tylewicz, U; Laghi, L; Dalla Rosa, M; Witrowa-Rajchert, D

2014-02-01

The present work investigates how ultrasound pretreatment modulates the effects of osmotic dehydration (OD) on the water state and microstructure of kiwifruit. Kiwifruit slices (10mm thick) were subjected to ultrasonic waves in a water bath at a frequency of 35 kHz for 10, 20 and 30 min. OD process was then carried out by immersing the samples in 61.5% sucrose solution equilibrated at 25°C for a contact period of 0, 10, 20, 30, 60 and 120 min. The partition of water into the cellular tissue structures (vacuole, cytoplasm, extracellular spaces and cell wall) was investigated by Time Domain Nuclear Magnetic Resonance (TD-NMR). In parallel, the microstructure of kiwifruits slices was examined using a Scanning Electron Microscope. The results showed that US pretreatment performed for more than 10 min had a positive effect on the mass exchange caused by osmotic dehydration. A creation of microchannels and an increase of the average cross-section area of cells were observed when the samples were pretreated with US before OD. TD-NMR showed a slight redistribution of water through the substructures of the cells, as a function of the length of the US pretreatment applied. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Cardiac effects of magnesium sulfate pretreatment on acute dichlorvos-induced organophosphate poisoning: an experimental study in rats.

PubMed

Gunay, Nurullah; Kekec, Zeynep; Demiryurek, Seniz; Kose, Ataman; Namiduru, Emine S; Gunay, Nahide E; Sari, Ibrahim; Demiryurek, Abdullah T

2010-02-01

Although atropine and oximes are traditionally used in the management of organophosphate poisoning, investigations have been directed to finding additional therapeutic approaches. Thus, the aim of this study was to evaluate the cardiac effects of magnesium sulfate pretreatment on dichlorvos intoxication in rats. Rats were randomly divided into three groups as control, dichlorvos, and magnesium sulfate groups. After 6 h of dichlorvos or corn oil (as a vehicle) injection, venous blood samples were collected, and cardiac tissue samples were obtained. Biochemical analyses were performed to measure some parameters on serum and cardiac tissue. Immunohistochemical analyses of apoptosis and inducible nitric oxide (NO) synthase showed no change in cardiac tissue. Serum cholinesterase levels were markedly depressed with dichlorvos, and further suppressed markedly with magnesium sulfate pretreatment. Although we have demonstrated that serum NO levels in dichlorvos and magnesium sulfate groups were lower than the control group, cardiac tissue NO levels in magnesium sulfate group were higher than the other two groups. Mortality was not significantly affected with magnesium sulfate pretreatment. Uncertainty still persists on the right strategies for the treatment of organophosphate acute poisoning; however, it was concluded that our results do not suggest that magnesium sulfate therapy is beneficial in the management of acute dichlorvos-induced organophosphate poisoning, and also further studies are required.

Drop-to-drop solvent microextraction coupled with gas chromatography/mass spectrometry for rapid determination of trimeprazine in urine and blood of rats: application to pharmacokinetic studies.

PubMed

Agrawal, Kavita; Wu, Hui-Fen

2007-01-01

A simple and rapid method based on drop-to-drop solvent microextraction (DDSME) coupled with gas chromatography/mass spectrometry (GC/MS) has been successfully applied for the pharmacokinetic studies of trimeprazine in 8 microL of urine and blood samples of rats. Several factors that influenced the extraction efficiency of DDSME, such as selection of organic solvent, extraction time, exposure volume of organic phase, addition of salt and pH, were optimized. Linearity was obtained over the concentration ranges of 0.2-10, 0.25-7.0 and 0.5-6.0 microg/mL with correlation coefficients of 0.998, 0.996 and 0.993 in deionized water, urine and blood samples of rats, respectively. The limits of detection (LODs) of trimeprazine were 0.05, 0.06 and 0.1 microg/mL in deionized water, urine and blood samples. The concentrations of trimeprazine obtained in urine and blood samples of rats were 0.21-1.25 and 2.72-0.22 microg/mL, respectively, after a single intravenous administration of this drug. The enrichment factors and LOD values obtained by DDSME coupled to GC/MS were compared with those of hollow fiber liquid-phase microextraction (HF-LPME) combined with GC/MS. We believe that this novel approach can be very useful in clinical application since only one microdrop of biological samples was required to perform the pharmacokinetic studies from rats, so the sample pretreatments for animal experiments can be very easy too. Copyright (c) 2007 John Wiley & Sons, Ltd.

Lignin triggers irreversible cellulase loss during pretreated lignocellulosic biomass saccharification.

PubMed

Gao, Dahai; Haarmeyer, Carolyn; Balan, Venkatesh; Whitehead, Timothy A; Dale, Bruce E; Chundawat, Shishir Ps

2014-01-01

Non-productive binding of enzymes to lignin is thought to impede the saccharification efficiency of pretreated lignocellulosic biomass to fermentable sugars. Due to a lack of suitable analytical techniques that track binding of individual enzymes within complex protein mixtures and the difficulty in distinguishing the contribution of productive (binding to specific glycans) versus non-productive (binding to lignin) binding of cellulases to lignocellulose, there is currently a poor understanding of individual enzyme adsorption to lignin during the time course of pretreated biomass saccharification. In this study, we have utilized an FPLC (fast protein liquid chromatography)-based methodology to quantify free Trichoderma reesei cellulases (namely CBH I, CBH II, and EG I) concentration within a complex hydrolyzate mixture during the varying time course of biomass saccharification. Three pretreated corn stover (CS) samples were included in this study: Ammonia Fiber Expansion(a) (AFEX™-CS), dilute acid (DA-CS), and ionic liquid (IL-CS) pretreatments. The relative fraction of bound individual cellulases varied depending not only on the pretreated biomass type (and lignin abundance) but also on the type of cellulase. Acid pretreated biomass had the highest levels of non-recoverable cellulases, while ionic liquid pretreated biomass had the highest overall cellulase recovery. CBH II has the lowest thermal stability among the three T. reesei cellulases tested. By preparing recombinant family 1 carbohydrate binding module (CBM) fusion proteins, we have shown that family 1 CBMs are highly implicated in the non-productive binding of full-length T. reesei cellulases to lignin. Our findings aid in further understanding the complex mechanisms of non-productive binding of cellulases to pretreated lignocellulosic biomass. Developing optimized pretreatment processes with reduced or modified lignin content to minimize non-productive enzyme binding or engineering pretreatment-specific, low-lignin binding cellulases will improve enzyme specific activity, facilitate enzyme recycling, and thereby permit production of cheaper biofuels.

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.

Determination of germanium by AAS in chloride-containing matrices.

PubMed

Anwari, M A; Abbasi, H U; Volkan, M; Ataman, O Y

1996-06-01

Interference effects of NaCl on the ET-AAS determination of Ge have been studied. The use of several matrix modifiers to alleviate this problem such as Ni and Zn perchlorates and nitrates, nitric acid, ammonium nitrate are reported. The stabilizing effect of Zn and Ni perchlorates allows the use of high pretreatment temperatures. NaCl is thus thermally volatilized from the atomizer by employing pretreatment temperatures higher than 1500 degrees C resulting in an improved sensitivity. Germanium levels in zinc plant slag samples, have been determined and compared to those obtained for the same samples spiked with NaCl with platform and wall atomization using nickel perchlorate as a matrix modifier. The results were compared with those from a hydride generation system equipped with a liquid nitrogen trap. The recoveries for germanium have been almost complete and amount to 99% for the original slag samples and 80% for 15% (w/w) NaCl containing spiked samples.

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

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®.

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.

Ozone pretreatment of olive mill wastewaters (OMW) and its effect on OMW biochemical methane potential (BMP).

PubMed

Tsintavi, E; Pontillo, N; Dareioti, M A; Kornaros, M

2013-01-01

The possibility of coupling a physicochemical pretreatment (ozonation) with a biological treatment (anaerobic digestion) was investigated for the case of olive mill wastewaters (OMW). Batch ozonation experiments were performed in a glass bubble reactor. The parameters which were tested included the ozone concentration in the inlet gas stream, the reactor temperature and the composition of the liquid medium in terms of raw or fractionated OMW used. In the sequel, ozone-pretreated OMW samples were tested for their biochemical methane potential (BMP) under mesophilic conditions and these results were compared to the BMP of untreated OMW. The ozonation process alone resulted in a 57-76% decrease of total phenols and a 5-18% decrease of total carbohydrates contained in OMW, depending on the experimental conditions. Nevertheless, the ozone-pretreated OMW exhibited lower chemical oxygen demand removal and methane production during BMP testing compared to the untreated OMW.

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.

The effect of plasma pre-treatment on NaHCO3 desizing of blended sizes on cotton fabrics

NASA Astrophysics Data System (ADS)

Li, Xuming; Qiu, Yiping

2012-03-01

The influence of the He/O2 atmospheric pressure plasma jet pre-treatment on subsequent NaHCO3 desizing of blends of starch phosphate and poly(vinyl alcohol) on cotton fabrics is investigated. Atomic force microscopy and scanning electron microscopy analysis indicate that the surface topography of the samples has significantly changed and the surface roughness increases with an increase in plasma exposure time. X-ray photoelectron spectroscopy analysis shows that a larger number of oxygen-containing polar groups are formed on the sized fabric surface after the plasma treatment. The results of the percent desizing ratio (PDR) indicate that the plasma pretreatment facilitated the blended sizes removal from the cotton fabrics in subsequent NaHCO3 treatment and the PDR increases with prolonging plasma treatment time. The plasma technology is a promising pretreatment for desizing of blended sizes due to dramatically reduced desizing time.

Synergism between ultrasonic pretreatment and white rot fungal enzymes on biodegradation of wheat chaff.

PubMed

Sabarez, Henry; Oliver, Christine Maree; Mawson, Raymond; Dumsday, Geoff; Singh, Tanoj; Bitto, Natalie; McSweeney, Chris; Augustin, Mary Ann

2014-11-01

Lignocellulosic biomass samples (wheat chaff) were pretreated by ultrasound (US) (40kHz/0.5Wcm(-2)/10min and 400kHz/0.5Wcm(-2)/10min applied sequentially) prior to digestion by enzyme extracts obtained from fermentation of the biomass with white rot fungi (Phanerochaete chrysosporium or Trametes sp.). The accessibility of the cellulosic components in wheat chaff was increased, as demonstrated by the increased concentration of sugars produced by exposure to the ultrasound treatment prior to enzyme addition. Pretreatment with ultrasound increased the concentration of lignin degradation products (guaiacol and syringol) obtained from wheat chaff after enzyme addition. In vitro digestibility of wheat chaff was also enhanced by the ultrasonics pretreatment in combination with treatment with enzyme extracts. Degradation was enhanced with the use of a mixture of the enzyme extracts compared to that for a single enzyme extract. Copyright © 2014. Published by Elsevier B.V.

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.

Carbon nanotube synthesis via the catalytic chemical vapor deposition of methane in the presence of iron, molybdenum, and iron-molybdenum alloy thin layer catalysts

NASA Astrophysics Data System (ADS)

Yahyazadeh, Arash; Khoshandam, Behnam

In this study, we documented the catalytic chemical vapor deposition synthesis of carbon nanotubes (CNTs) using ferrocene and molybdenum hexacarbonyl as catalyst nanoparticle precursors and methane as a nontoxic and economical carbon source for the first time. Field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, wavelength dispersive X-ray spectrometry and transmission electron microscopy of the thin layer catalyst as a simple and cost effective catalyst preparation after methane decomposition reaction, along with Fourier transform infrared spectroscopy and Raman spectroscopy confirmed the growth of CNTs, from bimetallic nanoparticles, which are converted into iron-molybdenum alloy nanoparticles at 700 °C for pretreatment by hydrogen after chemical vapor deposition of thin layers. An investigation of the weight percentages of the chemical elements present in the CNTs synthesized from iron-molybdenum catalyst using quartz sheet substrate at 750 °C, confirmed a significant carbon yield of 75.4% which represents high catalyst activity. Additionally, multi-walled carbon nanotubes (∼16-55 nm in diameter and 1.2 μm in length) were observed in the iron-molybdenum alloy sample after methane decomposition reaction at 750 °C for 35 min. To show the role of iron and molybdenum coated on silicon substrate as two thin layer catalysts, samples were considered for CNTs growth (diameter ∼47-69 nm) at 800 °C and 830 °C, respectively. Moreover, the effect of hydrogen pretreatment was evaluated in terms of active metal coating properly. The best graphitic structure due to Raman spectroscopy outcomes (ID/IG ratio) was obtained for iron coated on a quartz sheet, which was estimated at 0.8505. Thermogravimetric analysis proved the thermal stability of the synthesized CNTs using iron thin-layer catalyst up to 350 °C.

Methodology for enabling high-throughput simultaneous saccharification and fermentation screening of yeast using solid biomass as a substrate.

PubMed

Elliston, Adam; Wood, Ian P; Soucouri, Marie J; Tantale, Rachelle J; Dicks, Jo; Roberts, Ian N; Waldron, Keith W

2015-01-01

High-throughput (HTP) screening is becoming an increasingly useful tool for collating biological data which would otherwise require the employment of excessive resources. Second generation biofuel production is one such process. HTP screening allows the investigation of large sample sets to be undertaken with increased speed and cost effectiveness. This paper outlines a methodology that will enable solid lignocellulosic substrates to be hydrolyzed and fermented at a 96-well plate scale, facilitating HTP screening of ethanol production, whilst maintaining repeatability similar to that achieved at a larger scale. The results showed that utilizing sheets of biomass of consistent density (handbills), for paper, and slurries of pretreated biomass that could be pipetted allowed standardized and accurate transfers to 96-well plates to be achieved (±3.1 and 1.7%, respectively). Processing these substrates by simultaneous saccharification and fermentation (SSF) at various volumes showed no significant difference on final ethanol yields, either at standard shake flask (200 mL), universal bottle (10 mL) or 96-well plate (1 mL) scales. Substrate concentrations of up to 10% (w/v) were trialed successfully for SSFs at 1 mL volume. The methodology was successfully tested by showing the effects of steam explosion pretreatment on both oilseed rape and wheat straws. This methodology could be used to replace large shake flask reactions with comparatively fast 96-well plate SSF assays allowing for HTP experimentation. Additionally this method is compatible with a number of standardized assay techniques such as simple colorimetric, High-performance liquid chromatography (HPLC) and Nuclear magnetic resonance (NMR) spectroscopy. Furthermore this research has practical uses in the biorefining of biomass substrates for second generation biofuels and novel biobased chemicals by allowing HTP SSF screening, which should allow selected samples to be scaled up or studied in more detail.

Copper circuit patterning on polymer using selective surface modification and electroless plating

NASA Astrophysics Data System (ADS)

Park, Sang Jin; Ko, Tae-Jun; Yoon, Juil; Moon, Myoung-Woon; Oh, Kyu Hwan; Han, Jun Hyun

2017-02-01

We have examined a potential new and simple method for patterning a copper circuit on PET substrate by copper electroless plating, without the pretreatment steps (i.e., sensitization and activation) for electroless plating as well as the etching processes of conventional circuit patterning. A patterned mask coated with a catalyst material, Ag, for the reduction of Cu ions, is placed on a PET substrate. Subsequent oxygen plasma treatment of the PET substrate covered with the mask promotes the selective generation of anisotropic pillar- or hair-like nanostructures coated with co-deposited nanoparticles of the catalyst material on PET. After oxygen plasma treatment, a Cu circuit is well formed just by dipping the plasma-treated PET into a Cu electroless plating solution. By increasing the oxygen gas pressure in the chamber, the height of the nanostructures increases and the Ag catalyst particles are coated on not only the top but also the side surfaces of the nanostructures. Strong mechanical interlocking between the Cu circuit and PET substrate is produced by the large surface area of the nanostructures, and enhances peel strength. Results indicate this new simple two step (plasma surface modification and pretreatment-free electroless plating) method can be used to produce a flexible Cu circuit with good adhesion.

Microbial communities of biomethanization digesters fed with raw and heat pre-treated microalgae biomasses.

PubMed

Sanz, Jose Luis; Rojas, Patricia; Morato, Ana; Mendez, Lara; Ballesteros, Mercedes; González-Fernández, Cristina

2017-02-01

Microalgae biomasses are considered promising feedstocks for biofuel and methane productions. Two Continuously Stirred Tank Reactors (CSTR), fed with fresh (CSTR-C) and heat pre-treated (CSTR-T) Chlorella biomass were run in parallel in order to determine methane productions. The methane yield was 1.5 times higher in CSTR-T with regard to CSTR-C. Aiming to understand the microorganism roles within of the reactors, the sludge used as an inoculum (I), plus raw (CSTR-C) and heat pre-treated (CSTR-T) samples were analyzed by high-throughput pyrosequencing. The bacterial communities were dominated by Proteobacteria, Bacteroidetes, Chloroflexi and Firmicutes. Spirochaetae and Actinobacteria were only detected in sample I. Proteobacteria, mainly Alfaproteobacteria, were by far the dominant phylum within of the CSTR-C bioreactor. Many of the sequences retrieved were related to bacteria present in activated sludge treatment plants and they were absent after thermal pre-treatment. Most of the sequences affiliated to the Bacteroidetes were related to uncultured groups. Anaerolineaceae was the sole family found of the Chloroflexi phylum. All of the genera identified of the Firmicutes phylum carried out macromolecule hydrolysis and by-product fermentation. The proteolytic bacteria were prevalent over the saccharolytic microbes. The percentage of the proteolytic genera increased from the inoculum to the CSTR-T sample in a parallel fashion with an available protein increase owing to the high protein content of Chlorella. To relate the taxa identified by high-throughput sequencing to their functional roles remains a future challenge. Copyright © 2016 Elsevier Ltd. All rights reserved.

The effects of chemical and physical penetration enhancers on the percutaneous permeation of lidocaine through equine skin

PubMed Central

2014-01-01

Background The effect of physical and chemical permeation enhancers on in vitro transdermal permeation of lidocaine was investigated in the horse. Therefore, the effect of six vehicles (phosphate-buffered saline (PBS), 50% ethanol, 50% propylene glycol, 50% isopropylalcohol, 50% isopropylalcohol/isopropylmyristate and 50% dimethylsulfoxide) was examined as well as the effect of microneedle pretreatment with different needle lengths on transdermal drug delivery of lidocaine. The skin was obtained from the thorax of six Warmblood horses and was stored up to two weeks at - 20°C. Franz-type diffusion cells were used to study the transdermal permeation through split skin (600 μm thickness). The amount of lidocaine in the receptor fluid was determined by UV–VIS high-performance liquid chromatography. Results All investigated vehicle supplementations diminished the transdermal flux of lidocaine through equine skin in comparison to pure PBS except dimethylsulfoxide, which resulted in comparable permeation rates to PBS. The maximum flux (Jmax) was 1.6-1.8 fold lower for lidocaine applied in 50% ethanol, propylene glycol, isopropylalcohol and isopropylalcohol/isopropylmyristate. A significant higher Jmax of lidocaine was observed when lidocaine was applied in PBS onto microneedle pretreated skin with similar permeation rates in both needle lengths. After 6 hours, 1.7 fold higher recovery rates were observed in the microneedle pretreated skin samples than in the untreated control samples. The lagtimes were reduced to 20–50% in the microneedle pretreated skin samples. Conclusion Microneedles represent a promising tool for transdermal lidocaine application in the horse with a rapid systemic bioavailability. PMID:24950611

Transformation of oil palm fronds into pentose sugars using copper (II) sulfate pentahydrate with the assistance of chemical additive.

PubMed

Loow, Yu-Loong; Wu, Ta Yeong

2018-06-15

Among the chemical pretreatments available for pretreating biomass, the inorganic salt is considered to be a relatively new but simple reagent that offers comparable pentose (C5) sugar recoveries as the conventional dilute acid hydrolysis. This study investigated the effects of different concentrations (1.5-6.0% (v/v)) of H 2 O 2 or Na 2 S 2 O 8 in facilitating CuSO 4 ·5H 2 O pretreatment for improving pentose sugar recovery from oil palm fronds. The best result was observed when 0.2 mol/L of CuSO 4 ·5H 2 O was integrated with 4.5% (v/v) of Na 2 S 2 O 8 to recover 8.2 and 0.9 g/L of monomeric xylose and arabinose, respectively in the liquid fraction. On the other hand, an addition of 1.5% (v/v) of H 2 O 2 yielded approximately 74% lesser total pentose sugars as compared to using 4.5% (v/v) Na 2 S 2 O 8 . By using CuSO 4 ·5H 2 O alone (control), only 0.8 and 1.0 g/L xylose and arabinose, respectively could be achieved. The results mirrored the importance of using chemical additives together with the inorganic salt pretreatment of oil palm fronds. Thus, an addition of 4.5% (v/v) of Na 2 S 2 O 8 during CuSO 4 ·5H 2 O pretreatment of oil palm fronds at 120 °C and 30 min was able to attain a total pentose sugar yield up to ∼40%. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Manovic, V.; Anthony, E.J.; Loncarevic, D.

CaO-based looping cycles are promising processes for CO{sub 2} Capture from both syngas and flue gas. The technology is based on cyclical carbonation of CaO and regeneration of CaCO{sub 3} in a dual fluidized-bed reactor to produce a pure CO{sub 2} stream suitable for sequestration. Use of spent sorbent from CO{sub 2} looping cycles for SO{sub 2} capture is investigated. Three limestones were investigated: Kelly Rock (Canada), La Blanca (Spain), and Katowice (Poland, Upper Silesia). Carbonation/calcination cycles were performed in a tube furnace with both the original limestones and samples thermally pretreated for different times (i.e., sintered). The spent sorbentmore » samples were sulfated in a thermogravimetric analyzer (TGA). The changes in the resulting sorbent pore structure were then investigated using mercury porosimetry. It has been shown that the sulfation rates of both thermally pretreated and spent sorbent samples are lower in comparison with those of the original samples. However, final conversions of both spent and pretreated sorbents after longer sulfation time were comparable or higher than those observed for the original sorbents under comparable conditions. Maximum sulfation levels strongly depend on sorbent porosity and pore surface area. The results showed that spent sorbent samples from CO{sub 2} looping cycles can be used as sorbents for SO{sub 2} retention in cases where significant porosity loss does not occur during CO{sub 2} reaction cycles. In the case of spent Kelly Rock and Katowice samples, sorbent particles are practically uniformly sulfated, achieving final conversions that are determined by the total pore volume available for the bulky CaSO{sub 4} product.« less

The "Anatomy" of a Performance-Enhancing Drug Test in Sports

ERIC Educational Resources Information Center

Werner, T. C.

2012-01-01

The components of a performance-enhancing drug (PED) test in sports include sample selection, collection, establishing sample integrity, sample pretreatment, analyte detection, data evaluation, reporting results, and action taken based on the result. Undergraduate curricula generally focus on the detection and evaluation steps of an analytical…

Impact of PAC Fines in Fouling of Polymeric and Ceramic Low-Pressure Membranes for Drinking Water Treatment

PubMed Central

Oligny, Laurent; Bérubé, Pierre R.; Barbeau, Benoit

2016-01-01

This study assessed the issue of membrane fouling in a Hybrid Membrane Process (HMP) due to the export of powdered activated carbon (PAC) fines from a pretreatment contactor. Two parallel pilot-scale ceramic and polymeric membranes were studied. Reversible and irreversible foulings were measured following three cleaning procedures: Physical backwashing (BW), chemically enhanced backwashing (CEB) and Clean-in-Place (CIP). The impacts on fouling of membrane type, operation flux increase and the presence/absence of the PAC pretreatment were investigated. Membranes without pretreatment were operated in parallel as a control. In addition, CIP washwaters samples were analyzed to measure organic and inorganic foulants removed from the membranes. It was observed that for the polymeric membranes, fouling generally increased with the presence of the PAC pretreatment because of the export of fines. On the contrary, the ceramic membranes were not significantly impacted by their presence. The analysis of CIP washwaters showed a greater total organic carbon (TOC) content on membranes with a PAC pretreatment while no similar conclusion could be made for inorganic foulants. PMID:27399788

Improvement of anaerobic digestion of sewage sludge in a wastewater treatment plant by means of mechanical and thermal pre-treatments: Performance, energy and economical assessment.

PubMed

Ruffino, Barbara; Campo, Giuseppe; Genon, Giuseppe; Lorenzi, Eugenio; Novarino, Daniel; Scibilia, Gerardo; Zanetti, Mariachiara

2015-01-01

Performances of mechanical and low-temperature (<100°C) thermal pre-treatments were investigated to improve the present efficiency of anaerobic digestion (AD) carried out on waste activated sludge (WAS) in the largest Italian wastewater treatment plant (2,300,000p.e.). Thermal pre-treatments returned disintegration rates of one order of magnitude higher than mechanical ones (about 25% vs. 1.5%). The methane specific production increased by 21% and 31%, with respect to untreated samples, for treatment conditions of respectively 70 and 90°C, 3h. Thermal pre-treatments also decreased WAS viscosity. Preliminary energy and economic assessments demonstrated that a WAS final total solid content of 5% was enough to avoid the employment of auxiliary methane for the pre-treatment at 90°C and the subsequent AD process, provided that all the heat generated was transferred to WAS through heat exchangers. Moreover, the total revenues from sale of the electricity produced from biogas increased by 10% with respect to the present scenario. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

Gambling Disorder: Exploring Pre-treatment and In-treatment Dropout Predictors. A UK Study.

PubMed

Ronzitti, Silvia; Soldini, Emiliano; Smith, Neil; Clerici, Massimo; Bowden-Jones, Henrietta

2017-12-01

The aim of this study was to identify predictors of treatment dropout in a sample of gamblers attending a specialist clinic for gambling disorder. We analysed data on 846 treatment-seeking pathological gamblers. Firstly, we investigated differences in socio-demographic and clinical variables between treatment completers and pre-treatment dropouts, as well as between treatment completers and during-treatment dropouts. Subsequently, variables were entered into a multinomial logistic regression model to identify significant predictors of pre-treatment and in-treatment dropout. Overall, 44.8% of clients did not complete the treatment: 27.4% dropped out before starting it, while 17.4% dropped out during the treatment. Younger age and use of drugs were associated with pre-treatment dropout, while family history of gambling disorder, a lower PGSI score, and being a smoker were related with in-treatment dropout. Our findings suggest that pre-treatment dropouts differ from in-treatment dropouts, and, thus, further research will benefit from considering these groups separately. In addition, this newly gained knowledge will also be helpful in increasing treatment retention in specific subgroups of problem gamblers.

Impact of PAC Fines in Fouling of Polymeric and Ceramic Low-Pressure Membranes for Drinking Water Treatment.

PubMed

Oligny, Laurent; Bérubé, Pierre R; Barbeau, Benoit

2016-07-07

This study assessed the issue of membrane fouling in a Hybrid Membrane Process (HMP) due to the export of powdered activated carbon (PAC) fines from a pretreatment contactor. Two parallel pilot-scale ceramic and polymeric membranes were studied. Reversible and irreversible foulings were measured following three cleaning procedures: Physical backwashing (BW), chemically enhanced backwashing (CEB) and Clean-in-Place (CIP). The impacts on fouling of membrane type, operation flux increase and the presence/absence of the PAC pretreatment were investigated. Membranes without pretreatment were operated in parallel as a control. In addition, CIP washwaters samples were analyzed to measure organic and inorganic foulants removed from the membranes. It was observed that for the polymeric membranes, fouling generally increased with the presence of the PAC pretreatment because of the export of fines. On the contrary, the ceramic membranes were not significantly impacted by their presence. The analysis of CIP washwaters showed a greater total organic carbon (TOC) content on membranes with a PAC pretreatment while no similar conclusion could be made for inorganic foulants.

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.

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.

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.

Nanoliter-Scale Oil-Air-Droplet Chip-Based Single Cell Proteomic Analysis.

PubMed

Li, Zi-Yi; Huang, Min; Wang, Xiu-Kun; Zhu, Ying; Li, Jin-Song; Wong, Catherine C L; Fang, Qun

2018-04-17

Single cell proteomic analysis provides crucial information on cellular heterogeneity in biological systems. Herein, we describe a nanoliter-scale oil-air-droplet (OAD) chip for achieving multistep complex sample pretreatment and injection for single cell proteomic analysis in the shotgun mode. By using miniaturized stationary droplet microreaction and manipulation techniques, our system allows all sample pretreatment and injection procedures to be performed in a nanoliter-scale droplet with minimum sample loss and a high sample injection efficiency (>99%), thus substantially increasing the analytical sensitivity for single cell samples. We applied the present system in the proteomic analysis of 100 ± 10, 50 ± 5, 10, and 1 HeLa cell(s), and protein IDs of 1360, 612, 192, and 51 were identified, respectively. The OAD chip-based system was further applied in single mouse oocyte analysis, with 355 protein IDs identified at the single oocyte level, which demonstrated its special advantages of high enrichment of sequence coverage, hydrophobic proteins, and enzymatic digestion efficiency over the traditional in-tube system.

A high-throughput core sampling device for the evaluation of maize stalk composition

PubMed Central

2012-01-01

Background A major challenge in the identification and development of superior feedstocks for the production of second generation biofuels is the rapid assessment of biomass composition in a large number of samples. Currently, highly accurate and precise robotic analysis systems are available for the evaluation of biomass composition, on a large number of samples, with a variety of pretreatments. However, the lack of an inexpensive and high-throughput process for large scale sampling of biomass resources is still an important limiting factor. Our goal was to develop a simple mechanical maize stalk core sampling device that can be utilized to collect uniform samples of a dimension compatible with robotic processing and analysis, while allowing the collection of hundreds to thousands of samples per day. Results We have developed a core sampling device (CSD) to collect maize stalk samples compatible with robotic processing and analysis. The CSD facilitates the collection of thousands of uniform tissue cores consistent with high-throughput analysis required for breeding, genetics, and production studies. With a single CSD operated by one person with minimal training, more than 1,000 biomass samples were obtained in an eight-hour period. One of the main advantages of using cores is the high level of homogeneity of the samples obtained and the minimal opportunity for sample contamination. In addition, the samples obtained with the CSD can be placed directly into a bath of ice, dry ice, or liquid nitrogen maintaining the composition of the biomass sample for relatively long periods of time. Conclusions The CSD has been demonstrated to successfully produce homogeneous stalk core samples in a repeatable manner with a throughput substantially superior to the currently available sampling methods. Given the variety of maize developmental stages and the diversity of stalk diameter evaluated, it is expected that the CSD will have utility for other bioenergy crops as well. PMID:22548834

Effect of Porcelain Surface Pretreatments on Composite Resin-Porcelain Shear Bond Strength

DTIC Science & Technology

1991-05-01

Presented to the Faculty of The University of Texas Graduate School of Biomedical Sciences at San Antonio in Partial Fulfillment of the Requirements...Breckner III The University of Texas Graduate School of Biomedical Sciences at San Antonio Supervising Professor: Barry K. Norling, Ph.D. The bond between...necessary to pretreat the porcelain prior to luting. The samples were not, however, hydrated or thermally stressed . Sheth et al. (1988) supported the

Using the properties of soil to speed up the start-up process, enhance process stability, and improve the methane content and yield of solid-state anaerobic digestion of alkaline-pretreated poplar processing residues.

PubMed

Yao, Yiqing; Luo, Yang; Li, Tian; Yang, Yingxue; Sheng, Hongmei; Virgo, Nolan; Xiang, Yun; Song, Yuan; Zhang, Hua; An, Lizhe

2014-01-01

Solid-state anaerobic digestion (SS-AD) was initially adopted for the treatment of municipal solid waste. Recently, SS-AD has been increasingly applied to treat lignocellulosic biomass, such as agricultural and forestry residues. However, studies on the SS-AD process are few. In this study, the process performance and methane yield from SS-AD of alkaline-pretreated poplar processing residues (PPRs) were investigated using the properties of soil, such as buffering capacity and nutritional requirements. The results showed that the lignocellulosic structures of the poplar sample were effectively changed by NaOH pretreatment, as indicated by scanning electron microscopy and Fourier transform infrared spectra analysis. The start-up was markedly hastened, and the process stability was enhanced. After NaOH pretreatment, the maximum methane yield (96.1 L/kg volatile solids (VS)) was obtained under a poplar processing residues-to-soil sample (P-to-S) ratio of 2.5:1, which was 29.9% and 36.1% higher than that of PPRs (74.0 L/kg VS) and that of experiments without NaOH pretreatment (70.6 L/kg VS), respectively. During steady state, the increase in the methane content of the experiment with a P-to-S ratio of 2.5:1 was 4.4 to 50.9% higher than that of the PPRs. Degradation of total solids and volatile solids ranged from 19.3 to 33.0% and from 34.9 to 45.9%, respectively. The maximum reductions of cellulose and hemicellulose were 52.6% and 42.9%, respectively, which were in accordance with the maximal methane yield. T 80 for the maximum methane yield for the experiments with NaOH pretreatment was 11.1% shorter than that for the PPRs. Pretreatment with NaOH and addition of soil led to a significant improvement in the process performance and the methane yield of SS-AD of PPRs. The changes in lignocellulosic structures induced by NaOH pretreatment led to an increase in methane yield. For the purpose of practical applications, SS-AD with soil addition is a convenient, economical, and practical technique.

Sulphation of CaO-Based Sorbent Modified in CO2 Looping Cycles

NASA Astrophysics Data System (ADS)

Manovic, Vasilije; Anthony, Edward J.; Loncarevic, Davor

CaO-based looping cycles for CO2 capture at high temperatures are based on cyclical carbonation of CaO and regeneration of CaCO3. The main limitation of natural sorbents is the loss of carrying capacity with increasing numbers of reaction cycles, resulting in spent sorbent ballast. Use of spent sorbent from CO2 looping cycles for SO2 capture is a possible solution investigated in this study. Three limestones were investigated: Kelly Rock (Canada), La Blanca (Spain) and Katowice (Poland). Carbonation/calcination cycles were performed in a tube furnace with original limestones and samples thermally pretreated for different times (i.e., sintered). The spent sorbent samples were sulphated in a thermogravimetric analyzer. Changes in the resulting pore structure were then investigated using mercury porosimetry. Final conversions of both spent and pretreated sorbents after longer sulphation times were comparable or higher than those observed for the original sorbents. Maximum sulphation levels strongly depend on sorbent porosity and pore surface area. The shrinkage of sorbent particles during calcination/cycling resulted in a loss of sorbent porosity (≤48%), which corresponds to maximum sulphation levels ˜55% for spent Kelly Rock and Katowice. However, this is ˜10% higher than for the original samples. By contrast, La Blanca limestone had more pronounced particle shrinkage during pretreatment and cycling, leading to lower porosity, <35%, resulting in sulphation conversion of spent samples <30%, significantly lower than for the original sample (45%). These results showed that spent sorbent samples from CO2 looping cycles can be used as sorbents for SO2 retention if significant porosity loss does not occur during CO2 reaction cycles. For spent Kelly Rock and Katowice samples final conversions are determined by the total pore volume available for the bulky CaSO4 product.

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.

Simple Heat Treatment of Zirconia Ceramic Pre-Treated with Silane Primer to Improve Resin Bonding.

PubMed

Ha, Jung-Yun; Son, Jun Sik; Kim, Kyo-Han; Kwon, Tae-Yub

2015-01-01

Establishing a strong resin bond to dental zirconia ceramic remains difficult. Previous studies have shown that the conventional application of silane does not work well with zirconia. This paper reports that a silane pre-treatment of dental zirconia ceramic combined with subsequent heat treatment has potential as an adhesive cementation protocol for improving zirconia-resin bonding. Among the various concentrations (0.1 to 16 vol%) of experimental γ-methacryloxypropyltrimethoxysilane (γ-MPTS) primers assessed, the 1% solution was found to be the most effective in terms of the shear bond strength of the resin cement to dental zirconia ceramic. A high shear bond strength (approx. 30 MPa) was obtained when zirconia specimens were pre-treated with this primer and then heat-treated in a furnace for 60 min at 150 degrees C. Heat treatment appeared to remove the hydrophilic constituents from the silane film formed on the zirconia ceramic surface and accelerate the condensation reactions between the silanol groups of the hydrolyzed silane molecules at the zirconia/resin interface, finally making a more desirable surface for bonding with resin. This estimation was supported by Fourier transform infrared spectroscopy of the silanes prepared in this study.

Validation of a predictive model that identifies patients at high risk of developing febrile neutropaenia following chemotherapy for breast cancer.

PubMed

Jenkins, P; Scaife, J; Freeman, S

2012-07-01

We have previously developed a predictive model that identifies patients at increased risk of febrile neutropaenia (FN) following chemotherapy, based on pretreatment haematological indices. This study was designed to validate our earlier findings in a separate cohort of patients undergoing more myelosuppressive chemotherapy supported by growth factors. We conducted a retrospective analysis of 263 patients who had been treated with adjuvant docetaxel, adriamycin and cyclophosphamide (TAC) chemotherapy for breast cancer. All patients received prophylactic pegfilgrastim and the majority also received prophylactic antibiotics. Thirty-one patients (12%) developed FN. Using our previous model, patients in the highest risk group (pretreatment absolute neutrophil count≤3.1 10(9)/l and absolute lymphocyte count≤1.5 10(9)/l) comprised 8% of the total population and had a 33% risk of developing FN. Compared with the rest of the cohort, this group had a 3.4-fold increased risk of developing FN (P=0.001) and a 5.2-fold increased risk of cycle 1 FN (P<0.001). A simple model based on pretreatment differential white blood cell count can be applied to pegfilgrastim-supported patients to identify those who are at higher risk of FN.

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.

Characterization of Lignin Streams during Bionic Liquid-Based Pretreatment from Grass, Hardwood, and Softwood

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

Dutta, Tanmoy; Papa, Gabriella; Wang, Eileen

Delignification as a function of ionic liquid (IL) pretreatment has potential in terms of recovering and converting the fractionated lignin streams to renewable products. Renewable biogenic ionic liquids, or bionic liquids (eg. cholinium lysinate, ([Ch][Lys])), provide opportunities in terms of effective, economic and sustainable lignocellulosic biomass pretreatment. We have evaluated [Ch][Lys] pretreatment in terms of sugar and lignin yields for three different feedstocks: switchgrass, eucalyptus, and pine. Four lignin streams isolated during [Ch][Lys] pretreatment and enzymatic hydrolysis were comprehensively analyzed, tracking their changes in physical-chemical structures. We observed changes in major lignin linkages and lignin aromatics units (p-hydroxyphenyl (H), guaiacylmore » (G), and syringil (S)) that occurred during pretreatment. A compositional analysis of the different process streams and a comprehensive mass balance in conjunction with multiple analytical techniques (Nuclear Magnetic Resonance (NMR), Mass Spectroscopy, Fourier Transform Infrared Spectroscopy (FT-IR), Gel Permeation Chromatography (GPC)) is presented. Qualitative and quantitative analyses indicates that there are significantly more lignin-carbohydrate interactions for G-rich lignin in pine. The lignin removal and extent of lignin depolymerization for switchgrass and eucalyptus were higher than pine, and follows the order of switchgrass > eucalyptus > pine. The recovered lignin from pretreated liquid contained a lower relative amount of carbohydrate signals than raw biomass, indicating a high degree of dissociation of lignin carbohydrate complex (LCC) linkages for all samples analyzed. The insights gained from this work contribute to better understanding of physiochemical properties of lignin streams generated during [Ch][Lys] pretreatment, offering a starting point for lignin valorization strategies.« less

Low-temperature hydrothermal pretreatment followed by dry anaerobic digestion: A sustainable strategy for manure waste management regarding energy recovery and nutrients availability.

PubMed

Huang, Weiwei; Zhao, Ziwen; Yuan, Tian; Huang, Wenli; Lei, Zhongfang; Zhang, Zhenya

2017-12-01

This study evaluated the feasibility of low-temperature hydrothermal (HT) pretreatment for improving dry anaerobic digestion (AD) of swine manure (SM) and nutrient elements reclamation, with specific goals to minimize the drawbacks of conventional HT process including high energy consumption, inhibitory compounds formation and unfavorable pH/alkalinity decrease. Pretreatment at 110-130°C for holding 30min increased the soluble organic carbon (SOC) concentration in SM by 13-26%. After being mixed with inocula, the pretreated SM was applied for dry AD tests successfully without initial pH adjustment, achieving a CH 4 yield of 280.18-328.93ml/g-VS fed (14-34% increase compared to that from raw SM). Energy assessment indicated a positive net gain of 0.95kJ/g-VS by adopting HT pretreatment at 130°C. Except for increment in CH 4 yield, low-temperature HT pretreatment also promoted organic-N mineralization, increasing N fractions in the digestate available for plants. After 70days' dry AD, a high ammonia-N to total nitrogen (TN) ratio of 71% was obtained for the SM sample pretreated at 130°C, in sharp contrast to that of 38% in raw SM. P bioavailability in the final digestate was not greatly affected by the HT pretreatment since the labile organics were mostly degraded after AD, in which P existing forms were influenced by the multivalent metals content in SM. Overall, 23-27% of the total P was potentially bioavailable in all digestates. Copyright © 2017 Elsevier Ltd. All rights reserved.

Simple validated LC-MS/MS method for the determination of atropine and scopolamine in plasma for clinical and forensic toxicological purposes.

PubMed

Koželj, Gordana; Perharič, Lucija; Stanovnik, Lovro; Prosen, Helena

2014-08-05

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of atropine and scopolamine in 100μL human plasma was developed and validated. Sample pretreatment consisted of protein precipitation with acetonitrile followed by a concentration step. Analytes and levobupivacaine (internal standard) were separated on a Zorbax XDB-CN column (75mm×4.6mm i.d., 3.5μm) with gradient elution (purified water, acetonitrile, formic acid). The triple quadrupole MS was operated in ESI positive mode. Matrix effect was estimated for deproteinised plasma samples. Selected reaction monitoring (SRM) was used for quantification in the range of 0.10-50.00ng/mL. Interday precision for both tropanes and intraday precision for atropine was <10%, intraday precision for scopolamine was <14% and <18% at lower limit of quantification (LLOQ). Mean interday and intraday accuracies for atropine were within ±7% and for scopolamine within ±11%. The method can be used for determination of therapeutic and toxic levels of both compounds and has been successfully applied to a study of pharmacodynamic and pharmacokinetic properties of tropanes, where plasma samples of volunteers were collected at fixed time intervals after ingestion of a buckwheat meal, spiked with five low doses of tropanes. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of 15 polycyclic aromatic hydrocarbons in aquatic products by solid-phase extraction and GC-MS.

PubMed

Liu, Qiying; Guo, Yuanming; Sun, Xiumei; Hao, Qing; Cheng, Xin; Zhang, Lu

2018-02-22

We propose a method for the simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons in marine samples (muscle) employing gas chromatography with mass spectrometry after saponification with ultrasound-assisted extraction and solid-phase extraction. The experimental conditions were optimized by the response surface method. In addition, the effects of different lyes and extractants on polycyclic aromatic hydrocarbons extraction were discussed, and saturated sodium carbonate was first used as the primary saponification reaction and extracted with 10 mL of ethyl acetate and secondly 1 mol/L of sodium hydroxide and 10 mL of n-hexane were used to achieve better results. The average recovery was 67-112%. Satisfactory data showed that the method has good reproducibility with a relative standard deviation of <13%. The detection limits of polycyclic aromatic hydrocarbons were 0.02-0.13 ng/g. Compared with other methods, this method has the advantages of simple pretreatment, low solvent consumption, maximum polycyclic aromatic hydrocarbons extraction, the fast separation speed, and the high extraction efficiency. It is concluded that this method meets the batch processing requirements of the sample and can also be used to determine polycyclic aromatic hydrocarbons in other high-fat (fish, shrimp, crab, shellfish) biological samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Resonance Rayleigh scattering method for determination of 2-mercaptobenzothiazole using gold nanoparticles probe.

PubMed

Parham, Hooshang; Pourreza, Nahid; Marahel, Farzaneh

2015-01-01

A sensitive, simple and novel method was developed to determine 2-mercaptobenzothiazole (2MBT) in water samples. This method was based on the interaction between gold nanoparticles (AuNPs) and 2MBT followed by increasing of the resonance Rayleigh scattering (RRS) intensity of nanoparticles. The change in RRS intensity (ΔIRRS) was linearly correlated to the concentration of 2MBT over the ranges of 5.0-100.0 and 100.0-300.0 μg L(-1). 2MBT can be measured in a short time (5 min) without any complicated or time-consuming sample pretreatment process. Parameters that affect the RRS intensities such as pH, concentration of AuNPs, standing time, electrolyte concentration, and coexisting substances were systematically investigated and optimized. Interference tests showed that the developed method has a very good selectivity and could be used conveniently for determination of 2MBT. The limit of detection (LOD) and limit of quantification (LOQ) were 1.0 and 3.0 μg L(-1), respectively. Relative standard deviations (RSD) for 20.0 and 80.0 μg L(-1) of 2MBT were 1.1 and 2.3, respectively. Possible mechanisms for the RRS changes of AuNPs in the presence of 2MBT were discussed and the method was successfully applied for the analysis of real water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Targeted analysis and determination of β-agonists, hormones, glucocorticoid and psychiatric drugs in feed by liquid chromatography with electrospray ionization tandem mass spectrometry.

PubMed

Zhu, Yufei; Xie, Shuyu; Chen, Dongmei; Pan, Yuanhu; Qu, Wei; Wang, Xu; Liu, Zhenli; Peng, Dapeng; Huang, Lingli; Tao, Yanfei; Yuan, Zonghui

2016-07-01

A comprehensive strategy combining a quantitative method was developed for 30 banned drugs including β-agonists, hormones, glucocorticoid and psychiatric drugs in swine and chicken feeds. This rapid, simple and effective extraction method was based on matrix solid-phase dispersion and electrospray ionization tandem mass spectrometry. The quantitative method was validated after previous statistical optimization of the main parameters of matrix solid-phase dispersion. The limit of quantification of dopamine hydrochloride, chlormadinone acetate, melengestrol acetate, testosterone propionate, nandrolone and midazolam was 2 μg/kg and that of the other 24 drugs was 1 μg/kg. The recoveries of β-agonists, hormones, glucocorticoid and psychiatric drugs spiked in swine and chicken feeds at a concentration range of 1-8 μg/kg were above 70.1% with inter-day relative standard deviations less than 15.8%. The analytical strategy was applied to 100 feed samples collected from a local market in Wuhan (China). Clenbuterol, ractopamine and melengestrol acetate were identified and quantified at the level 0.2∼3.5 μg/kg. The rapid and reliable method can be used to efficiently separate, characterize and quantify the residues of 30 banned drugs in swine and chicken feeds with advantages of simple pretreatment and environmental friendly nature. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

PubMed

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in biological or environmental samples. Due to low consumption of eluent (usually 0.3-1mL/run) mainly composed of water-alcohol binary mixtures, this method can be considered as environmentally friendly and green chemistry focused analytical tool, supplementary to analytical protocols involving column chromatography or planar micro-fluidic devices. Copyright © 2011 Elsevier Ltd. All rights reserved.

Identification of the time-point which gives a plasma rabeprazole concentration that adequately reflects the area under the concentration-time curve.

PubMed

Niioka, Takenori; Uno, Tsukasa; Yasui-Furukori, Norio; Shimizu, Mikiko; Sugawara, Kazunobu; Tateishi, Tomonori

2006-10-01

The purpose of this study is to evaluate whether a simple formula using limited blood samples can predict the area under the plasma rabeprazole concentration-time curve (AUC) in co-administration with CYP inhibitors. A randomized double-blind placebo-controlled crossover study design in three phases was conducted at intervals of 2 weeks. Twenty-one healthy Japanese volunteers, including three CYP2C19 genotype groups, took a single oral 20-mg dose of rabeprazole after three 6-day pretreatments, i.e., clarithromycin 800 mg/day, fluvoxamine 50 mg/day, and placebo. Prediction formulas of the AUC were derived from pharmacokinetics data of 21 subjects in three phases using multiple linear regression analysis. Ten blood samples were collected over 24 h to calculate AUC. Plasma concentrations of rabeprazole was measured by an HPLC-assay (l.l.q.=1 ng/ml). The AUC was based on all the data sets (n=63). The linear regression using two points (C3 and C6) could predict AUC(0-infinity) precisely, irrespective of CYP2C19 genotypes and CYP inhibitors (AUC(0-infinity)=1.39xC3+7.17xC6+344.14, r (2)=0.825, p<0.001). The present study demonstrated that the AUC of rabeprazole can be estimated by the simple formula using two-point concentrations. This formula can be more accurate for the prediction of AUC estimation than that reflected by CYP2C19 genotypes without any determination, even if there are significant differences for the CYP2C19 genotypes. Therefore, this prediction formula might be useful to evaluate whether CYP2C19 genotypes really reflects the curative effect of rabeprazole.

Liquid-liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel.

PubMed

Pereira, Andréia C; Rocha, Fábio R P

2014-06-04

A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I3(-) reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I2/100 g with a detection limit of 5 g I2/100 g. A coefficient of variation of 1.7% (n=10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I2 per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel. Copyright © 2014. Published by Elsevier B.V.

Magnetic bead and gold nanoparticle probes based immunoassay for β-casein detection in bovine milk samples.

PubMed

Li, Y S; Meng, X Y; Zhou, Y; Zhang, Y Y; Meng, X M; Yang, L; Hu, P; Lu, S Y; Ren, H L; Liu, Z S; Wang, X R

2015-04-15

In this work, a double-probe based immunoassay was developed for rapid and sensitive determination of β-casein in bovine milk samples. In the method, magnetic beads (MBs), employed as supports for the immobilization of anti-β-casein polyclonal antibody (PAb), were used as the capture probe. Colloidal gold nanoparticles (AuNPs), employed as a bridge for loading anti-β-casein monoclonal antibody (McAb) and horseradish peroxidase (HRP), were used as the amplification probe. The presence of β-casein causes the sandwich structures of MBs-PAb-β-casein-McAb-AuNPs through the interaction between β-casein and the anti-β-casein antibodies. The HRP, used as an enzymatic-amplified tracer, can catalytically oxidize the substrate 3,3',5,5'-tetramethylbenzidine (TMB), generating optical signals that are proportional to the quantity of β-casein. The linear range of the immunoassay was from 6.5 to 1520ngmL(-1). The limit of detection (LOD) was 4.8ngmL(-1) which was 700 times lower than that of MBs-antibody-HRP based immunoassay and 6-7 times lower than that from the microplate-antibody-HRP based assay. The recoveries of β-casein from bovine milk samples were from 95.0% to 104.3% that had a good correlation coefficient (R(2)=0.9956) with those obtained by an official standard Kjeldahl method. For higher sensitivity, simple sample pretreatment and shorter time requirement of the antigen-antibody reaction, the developed immunoassay demonstrated the viability for detection of β-casein in bovine milk samples. Copyright © 2014. Published by Elsevier B.V.

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by high-performance liquid chromatography with ultraviolet detection and liquid chromatography-tandem mass spectrometry for the determination of triclosan and 2,4-dichlorophenol in water samples.

PubMed

Zheng, Cao; Zhao, Jing; Bao, Peng; Gao, Jin; He, Jin

2011-06-24

A novel, simple and efficient dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) technique coupled with high-performance liquid chromatography with ultraviolet detection (HPLC-UV) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of triclosan and its degradation product 2,4-dichlorophenol in real water samples. The extraction solvent used in this work is of low density, low volatility, low toxicity and proper melting point around room temperature. The extractant droplets can be collected easily by solidifying it at a lower temperature. Parameters that affect the extraction efficiency, including type and volume of extraction solvent and dispersive solvent, salt effect, pH and extraction time, were investigated and optimized in a 5 mL sample system by HPLC-UV. Under the optimum conditions (extraction solvent: 12 μL of 1-dodecanol; dispersive solvent: 300 of μL acetonitrile; sample pH: 6.0; extraction time: 1 min), the limits of detection (LODs) of the pretreatment method combined with LC-MS/MS were in the range of 0.002-0.02 μg L(-1) which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Wide linearities, good precisions and satisfactory relative recoveries were also obtained. The proposed technique was successfully applied to determine triclosan and 2,4-dichlorophenol in real water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

In situ micro-spectroscopic investigation of lignin in poplar cell walls pretreated by maleic acid

DOE PAGES

Zeng, Yining; Zhao, Shuai; Wei, Hui; ...

2015-08-27

In higher plant cells, lignin provides necessary physical support for plant growth and resistance to attack by microorganisms. For the same reason, lignin is considered to be a major impediment to the process of deconstructing biomass to simple sugars by hydrolytic enzymes. Furthermore, the in situ variation of lignin in plant cell walls is important for better understanding of the roles lignin play in biomass recalcitrance.

Evaluation of Multiple Immunoassay Technology Platforms to Select the Anti-Drug Antibody Assay Exhibiting the Most Appropriate Drug and Target Tolerance

PubMed Central

Collet-Brose, Justine

2016-01-01

The aim of this study was, at the assay development stage and thus with an appropriate degree of rigor, to select the most appropriate technology platform and sample pretreatment procedure for a clinical ADA assay. Thus, ELISA, MSD, Gyrolab, and AlphaLISA immunoassay platforms were evaluated in association with target depletion and acid dissociation sample pretreatment steps. An acid dissociation step successfully improved the drug tolerance for all 4 technology platforms and the required drug tolerance was achieved with the Gyrolab and MSD platforms. The target tolerance was shown to be better for the ELISA format, where an acid dissociation treatment step alone was sufficient to achieve the desired target tolerance. However, inclusion of a target depletion step in conjunction with the acid treatment raised the target tolerance to the desired level for all of the technologies. A higher sensitivity was observed for the MSD and Gyrolab assays and the ELISA, MSD, and Gyrolab all displayed acceptable interdonor variability. This study highlights the usefulness of evaluating the performance of different assay platforms at an early stage in the assay development process to aid in the selection of the best fit-for-purpose technology platform and sample pretreatment steps. PMID:27243038

Ultrasound pretreatment of filamentous algal biomass for enhanced biogas production.

PubMed

Lee, Kwanyong; Chantrasakdakul, Phrompol; Kim, Daegi; Kong, Mingeun; Park, Ki Young

2014-06-01

The filamentous alga Hydrodictyon reticulatum harvested from a bench-scale wastewater treatment pond was used to evaluate biogas production after ultrasound pretreatment. The effects of ultrasound pretreatment at a range of 10-5000 J/mL were tested with harvested H. reticulatum. Cell disruption by ultrasound was successful and showed a higher degree of disintegration at a higher applied energy. The range of 10-5000 J/mL ultrasound was able to disintegrated H. reticulatum and the soluble COD was increased from 250 mg/L to 1000 mg/L at 2500 J/mL. The disintegrated algal biomass was digested for biogas production in batch experiments. Both cumulative gas generation and volatile solids reduction data were obtained during the digestion. Cell disintegration due to ultrasound pretreatment increased the specific biogas production and degradation rates. Using the ultrasound approach, the specific methane production at a dose of 40 J/mL increased up to 384 mL/g-VS fed that was 2.3 times higher than the untreated sample. For disintegrated samples, the volatile solids reduction was greater with increased energy input, and the degradation increased slightly to 67% at a dose of 50 J/mL. The results also indicate that disintegration of the algal cells is the essential step for efficient anaerobic digestion of algal biomass. Copyright © 2013 Elsevier Ltd. All rights reserved.

Transport and fate of organic wastes in groundwater at the Stringfellow hazardous waste disposal site, southern California

USGS Publications Warehouse

Leenheer, J.A.; Hsu, J.; Barber, L.B.

2001-01-01

In January 1999, wastewater influent and effluent from the pretreatment plant at the Stringfellow hazardous waste disposal site were sampled along with groundwater at six locations along the groundwater contaminant plume. The objectives of this sampling and study were to identify at the compound class level the unidentified 40-60% of wastewater organic contaminants, and to determine what organic compound classes were being removed by the wastewater pretreatment plant, and what organic compound classes persisted during subsurface waste migration. The unidentified organic wastes are primarily chlorinated aromatic sulfonic acids derived from wastes from DDT manufacture. Trace amounts of EDTA and NTA organic complexing agents were discovered along with carboxylate metabolites of the common alkylphenolpolyethoxylate plasticizers and nonionic surfactants. The wastewater pretreatment plant removed most of the aromatic chlorinated sulfonic acids that have hydrophobic neutral properties, but the p-chlorobenzenesulfonic acid which is the primary waste constituent passed through the pretreatment plant and was discharged in the treated wastewaters transported to an industrial sewer. During migration in groundwater, p-chlorobenzenesulfonic acid is removed by natural remediation processes. Wastewater organic contaminants have decreased 3- to 45-fold in the groundwater from 1985 to 1999 as a result of site remediation and natural remediation processes. The chlorinated aromatic sulfonic acids with hydrophobic neutral properties persist and have migrated into groundwater that underlies the adjacent residential community. Copyright ?? 2001 .

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.

Effect of thermal pre-treatment on the availability of PAHs for successive chemical oxidation in contaminated soils.

PubMed

Usman, M; Chaudhary, A; Biache, C; Faure, P; Hanna, K

2016-01-01

This is the premier study designed to evaluate the impact of thermal pre-treatment on the availability of polycyclic aromatic hydrocarbons (PAHs) for successive removal by chemical oxidation. Experiments were conducted in two soils having different PAH distribution originating from former coking plant sites (Homécourt, H, and Neuves Maisons, NM) located in northeast of France. Soil samples were pre-heated at 60, 100, and 150 °C for 1 week under inert atmosphere (N2). Pre-heating resulted in slight removal of PAHs (<10%) and loss of extractable organic matter (EOM). Then, these pre-heated soil samples were subjected to Fenton-like oxidation (H2O2 and magnetite) at room temperature. Chemical oxidation in soil without any pre-treatment showed almost no PAH degradation underscoring the unavailability of PAHs. However, chemical oxidation in pre-heated soils showed significant PAH degradation (19, 29, and 43% in NM soil and 31, 36, and 47% in H soil pre-treated at 60, 100, and 150 °C, respectively). No preferential removal of PAHs was observed after chemical oxidation in both soils. These results indicated the significant impact of pre-heating temperature on the availability of PAHs in contaminated soils and therefore may have strong implications in the remediation of contaminated soils especially where pollutant availability is a limiting factor.

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.

New radiocarbon measurement methods in the Hertelendi Laboratory, Hungary

NASA Astrophysics Data System (ADS)

Janovics, Róbert; Major, István; Rinyu, László; Veres, Mihály; Molnár, Mihály

2013-04-01

In this paper we present two very different and novel methods for C-14 measurement from dissolved inorganic carbonate (DIC) of water samples. A new LSC sample preparation method for liquid scintillation C-14 measurements was implemented in the ATOMKI. The first method uses direct absorption into a special absorbent (Carbosorb E®) and a following liquid scintillation measurement. Typical sample size is 20-40 litre of water. The developed CO2 absorption method is fast, and simple. The C-14 activities is measured by an ultra low background LSC (TRI-CARB 3170 TR/SL, Perkin Elmer) including quenching parameter (tSIE).The corresponding limit of C-14 dating is 31200 year. Several tests were executed with old borehole CO2 gas without significant content of C-14 and also performed on samples of known C-14 activities between 29 and 7000 pMC, previously measured by GPC. The combined uncertainty of the described determination is about 2 % in the case of recent carbon. It is a very cost-effective and easy to use method based on a novel and simple static absorption process for the CO2 extracted from groundwater. The other very sensitive method is based on accelerator mass spectrometry (AMS) using gas ion source. This method does not require graphite generation and a small volume of water sample (1-20mL) is enough for the radiocarbon measurement. The procedure is very similar to pre-treatment of carbonate contained sample preparation for stable isotope measurement with gasbench technique. We applied a MICADAS type accelerator mass spectrometry (AMS) with gas ion source for C-14 analysis. The radiocarbon content of water was sat free with phosphoric acid and then the headspace gas was rinsed vials. The whole measurement needs only 20 min of each sample. The precision of measurement is better than 1% for modern samples. The preparation is vastly reduced compared to the other AMS methods and principally allows fully automated measurements of groundwater samples with an auto-sampler. The presented two new methods can be suitable for C-14 measurements and dating of hydrological, and environmental samples as well. The new AMS facility in ATOMKI (Debrecen, Hungary) using an EnvironMICADAS AMS system with gas ion source has a great potential in groundwater C-14 analyses. The research was supported by the by TÁMOP-4.2.2.A-11/1/KONV and the Hungarian NSF (OTKA MB08-A 81515)

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.

Lignocellulosic ethanol production by starch-base industrial yeast under PEG detoxification

PubMed Central

Liu, Xiumei; Xu, Wenjuan; Mao, Liaoyuan; Zhang, Chao; Yan, Peifang; Xu, Zhanwei; Zhang, Z. Conrad

2016-01-01

Cellulosic ethanol production from lignocellulosic biomass offers a sustainable solution for transition from fossil based fuels to renewable alternatives. However, a few long-standing technical challenges remain to be addressed in the development of an economically viable fermentation process from lignocellulose. Such challenges include the needs to improve yeast tolerance to toxic inhibitory compounds and to achieve high fermentation efficiency with minimum detoxification steps after a simple biomass pretreatment. Here we report an in-situ detoxification strategy by PEG exo-protection of an industrial dry yeast (starch-base). The exo-protected yeast cells displayed remarkably boosted vitality with high tolerance to toxic inhibitory compounds, and with largely improved ethanol productivity from crude hydrolysate derived from a pretreated lignocellulose. The PEG chemical exo-protection makes the industrial S. cerevisiae yeast directly applicable for the production of cellulosic ethanol with substantially improved productivity and yield, without of the need to use genetically modified microorganisms. PMID:26837707