A SIMPLE AND FAST EXTRACTION METHOD FOR ORGANOCHLORINE PESTICIDES AND POLYCHLORINATED BIPHENYLS IN SMALL VOLUMES OF AVIAN SERUM

EPA Science Inventory

A solid-phase extraction (SPE) method was developed using 8 M urea to desorb and extract organochlorine pesticides (OCs) and polychlorinated biphenyls (PCBs) from avian serum for analysis by capillary gas chromatography with electron capture detection (GC-ECD). The analytes were ...

Rapid and simple immunochemical screening combined with hand-shaking extraction for thiamethoxam residue in agricultural products.

PubMed

Watanabe, Eiki; Kobara, Yuso; Miyake, Shiro

2013-06-01

With the aim of expanding the applicability of a kit-based enzyme-linked immunosorbent assay (ELISA) for the neonicotinoid insecticide thiamethoxam, the ELISA was newly applied to three kinds of agricultural samples (green pepper, eggplant and spinach). To offer the ELISA as a screening analysis for thiamethoxam residues, a rapid and simple method of extraction by hand-shaking was used, and speed-up and simplification of the sample treatment before the ELISA analysis were examined. Finally, the validity of the ELISA combined with the proposed extraction method was verified against a reference high-performance liquid chromatography (HPLC) method using real-world agricultural samples. There were no marked matrix effects derived from green pepper and eggplant extracts. On the other hand, although the effect due to a pigment in spinach extract on the assay performance was significant, it was effectively avoided by increasing the dilution level of the spinach extract. For thiamethoxam-spiked samples, acceptable recoveries of 97.9-109.1% and coefficients of variation of 0.3-11.5% were obtained. Inspection of the validity of the ELISA by comparison with the reference HPLC method showed that the two analytical results were very similar, and a high correlation was found between them (r>0.997). The evaluated ELISA combined with hand-shaking extraction provided a rapid and simple screening analysis that was quantitative and reliable for the detection of thiamethoxam in complex agricultural products. © 2012 Society of Chemical Industry.

A simple method for the extraction and identification of light density microplastics from soil.

PubMed

Zhang, Shaoliang; Yang, Xiaomei; Gertsen, Hennie; Peters, Piet; Salánki, Tamás; Geissen, Violette

2018-03-01

This article introduces a simple and cost-saving method developed to extract, distinguish and quantify light density microplastics of polyethylene (PE) and polypropylene (PP) in soil. A floatation method using distilled water was used to extract the light density microplastics from soil samples. Microplastics and impurities were identified using a heating method (3-5s at 130°C). The number and size of particles were determined using a camera (Leica DFC 425) connected to a microscope (Leica wild M3C, Type S, simple light, 6.4×). Quantification of the microplastics was conducted using a developed model. Results showed that the floatation method was effective in extracting microplastics from soils, with recovery rates of approximately 90%. After being exposed to heat, the microplastics in the soil samples melted and were transformed into circular transparent particles while other impurities, such as organic matter and silicates were not changed by the heat. Regression analysis of microplastics weight and particle volume (a calculation based on image J software analysis) after heating showed the best fit (y=1.14x+0.46, R 2 =99%, p<0.001). Recovery rates based on the empirical model method were >80%. Results from field samples collected from North-western China prove that our method of repetitive floatation and heating can be used to extract, distinguish and quantify light density polyethylene microplastics in soils. Microplastics mass can be evaluated using the empirical model. Copyright © 2017 Elsevier B.V. All rights reserved.

Polyamines and inorganic ions extracted from woody tissues by freeze-thawing

Treesearch

Rakesh Minocha; Walter C. Shortle

1994-01-01

A simple and fast method for extraction of major inorganic ions (Ca, Mg, Mn, K, and P) and cellular polyamines from small quantities of wood and woody plant tissues is described. The method involves repeated freezing and thawing of samples instead of homogenization or wet ash digestion. The efficiency of extraction of both polyamines and inorganic ions by these methods...

Vitamin K

USDA-ARS?s Scientific Manuscript database

A wide range of analytical techniques are available for the detection, quantitation, and evaluation of vitamin K in foods. The methods vary from simple to complex depending on extraction, separation, identification and detection of the analyte. Among the extraction methods applied for vitamin K anal...

Theoretical analysis of a method for extracting the phase of a phase-amplitude modulated signal generated by a direct-modulated optical injection-locked semiconductor laser

NASA Astrophysics Data System (ADS)

Lee, Hwan; Cho, Jun-Hyung; Sung, Hyuk-Kee

2017-05-01

The phase modulation (PM) and amplitude modulation (AM) of optical signals can be achieved using a direct-modulated (DM) optical injection-locked (OIL) semiconductor laser. We propose and theoretically analyze a simple method to extract the phase component of a PM signal produced by a DM-OIL semiconductor laser. The pure AM component of the combined PM-AM signal can be isolated by square-law detection in a photodetector and can then be used to compensate for the PM-AM signal based on an optical homodyne method. Using the AM compensation technique, we successfully developed a simple and cost-effective phase extraction method applicable to the PM-AM optical signal of a DM-OIL semiconductor laser.

[Studies on extraction process optimization of patrinia scabra Bunge saponins].

PubMed

Wang, Xue-Xi; Chen, Ru; Li, Shi-Gang; Shen, Wei; Cheng, Wei-Dong; Zhao, Jian-Xiong

2007-05-01

To optimize the conditions for the extraction of Patrinia scabra Bunge saponins. Orthogonal experimental design and ultrasonic method were employed to examine the conditions for the extraction by determination of saponins. The optimun condition for the extraction of Patrinia scabra Bunge saponins was as follows: 65% ethanol for 40 minutes, 55 degrees C and 210 watt of ultrasonic efficinecy. The extraction method of Patrinia scabra Bunge sponins is simple and efficient.

Calculating the Degradation Rate of Individual Proteins Using Xenopus Extract Systems.

PubMed

McDowell, Gary S; Philpott, Anna

2018-05-16

The Xenopus extract system has been used extensively as a simple, quick, and robust method for assessing the stability of proteins against proteasomal degradation. In this protocol, methods are provided for assessing the half-life of in vitro translated radiolabeled proteins using Xenopus egg or embryo extracts. © 2019 Cold Spring Harbor Laboratory Press.

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.

Comparison of six simple methods for extracting ribosomal and mitochondrial DNA from Toxocara and Toxascaris nematodes.

PubMed

Mikaeili, F; Kia, E B; Sharbatkhori, M; Sharifdini, M; Jalalizand, N; Heidari, Z; Zarei, Z; Stensvold, C R; Mirhendi, H

2013-06-01

Six simple methods for extraction of ribosomal and mitochondrial DNA from Toxocara canis, Toxocara cati and Toxascaris leonina were compared by evaluating the presence, appearance and intensity of PCR products visualized on agarose gels and amplified from DNA extracted by each of the methods. For each species, two isolates were obtained from the intestines of their respective hosts: T. canis and T. leonina from dogs, and T. cati from cats. For all isolates, total DNA was extracted using six different methods, including grinding, boiling, crushing, beating, freeze-thawing and the use of a commercial kit. To evaluate the efficacy of each method, the internal transcribed spacer (ITS) region and the cytochrome c oxidase subunit 1 (cox1) gene were chosen as representative markers for ribosomal and mitochondrial DNA, respectively. Among the six DNA extraction methods, the beating method was the most cost effective for all three species, followed by the commercial kit. Both methods produced high intensity bands on agarose gels and were characterized by no or minimal smear formation, depending on gene target; however, beating was less expensive. We therefore recommend the beating method for studies where costs need to be kept at low levels. Copyright © 2013 Elsevier Inc. All rights reserved.

Extraction and identification of cyclobutanones from irradiated cheese employing a rapid direct solvent extraction method.

PubMed

Tewfik, Ihab

2008-01-01

2-Alkylcyclobutanones (cyclobutanones) are accepted as chemical markers for irradiated foods containing lipid. However, current extraction procedures (Soxhlet-florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to gas chromatography-mass spectrophotometry identification. This paper outlines an alternative isolation and clean-up method for the extraction of cyclobutanones in irradiated Camembert cheese. The newly developed direct solvent extraction method enables the efficient screening of large numbers of food samples and is not as resource intensive as the BS EN 1785:1997 method. Direct solvent extraction appears to be a simple, robust method and has the added advantage of a considerably shorter extraction time for the analysis of foods containing lipid.

Antifouling booster biocide extraction from marine sediments: a fast and simple method based on vortex-assisted matrix solid-phase extraction.

PubMed

Caldas, Sergiane Souza; Soares, Bruno Meira; Abreu, Fiamma; Castro, Ítalo Braga; Fillmann, Gilberto; Primel, Ednei Gilberto

2018-03-01

This paper reports the development of an analytical method employing vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of diuron, Irgarol 1051, TCMTB (2-thiocyanomethylthiobenzothiazole), DCOIT (4,5-dichloro-2-n-octyl-3-(2H)-isothiazolin-3-one), and dichlofluanid from sediment samples. Separation and determination were performed by liquid chromatography tandem-mass spectrometry. Important MSPD parameters, such as sample mass, mass of C18, and type and volume of extraction solvent, were investigated by response surface methodology. Quantitative recoveries were obtained with 2.0 g of sediment sample, 0.25 g of C18 as the solid support, and 10 mL of methanol as the extraction solvent. The MSPD method was suitable for the extraction and determination of antifouling biocides in sediment samples, with recoveries between 61 and 103% and a relative standard deviation lower than 19%. Limits of quantification between 0.5 and 5 ng g -1 were obtained. Vortex-assisted MPSD was shown to be fast and easy to use, with the advantages of low cost and reduced solvent consumption compared to the commonly employed techniques for the extraction of booster biocides from sediment samples. Finally, the developed method was applied to real samples. Results revealed that the developed extraction method is effective and simple, thus allowing the determination of biocides in sediment samples.

A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

PubMed

Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

2016-06-01

In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparative separation and purification of steroidal saponins in Paris polyphylla var. yunnanensis by macroporous adsorption resins.

PubMed

Liu, Zhen; Wang, Jieyin; Gao, Wenyuan; Man, Shuli; Wang, Ying; Liu, Changxiao

2013-07-01

Saponins are active compounds in natural products. Many researchers have tried to find the method for knowing their concentration in herbs. Some methods, such as solid-liquid extraction and solvent extraction, have been developed. However, the extraction methods of the steroidal saponins from Paris polyphylla Smith var. yunnanensis (Liliaceae) are not fully researched. To establish a simple extraction method for the separation of steroidal saponins from the rhizomes of P. polyphylla Smith var. yunnanensis. Macroporous adsorption resins were used for the separation of steroidal saponins. To select the most suitable resins, seven kinds of macroporous resins were selected in this study. The static adsorption and desorption tests on macroporous resins were determined. Also, we optimized the temperature and the ethanol concentration in the extraction method by the contents of five kinds of saponins. Then, we compared the extraction method with two other methods. D101 resin demonstrated the best adsorption and desorption properties for steroidal saponins. Its adsorption data fits best to the Freundlich adsorption model. The contents of steroidal saponins in the product were 4.83-fold increased with recovery yields of 85.47%. The process achieved simple and effective enrichment and separation for steroidal saponins. The method provides a scientific basis for large-scale preparation of steroidal saponins from the Rhizoma Paridis and other plants.

Comparison of Two Simplification Methods for Shoreline Extraction from Digital Orthophoto Images

NASA Astrophysics Data System (ADS)

Bayram, B.; Sen, A.; Selbesoglu, M. O.; Vārna, I.; Petersons, P.; Aykut, N. O.; Seker, D. Z.

2017-11-01

The coastal ecosystems are very sensitive to external influences. Coastal resources such as sand dunes, coral reefs and mangroves has vital importance to prevent coastal erosion. Human based effects also threats the coastal areas. Therefore, the change of coastal areas should be monitored. Up-to-date, accurate shoreline information is indispensable for coastal managers and decision makers. Remote sensing and image processing techniques give a big opportunity to obtain reliable shoreline information. In the presented study, NIR bands of seven 1:5000 scaled digital orthophoto images of Riga Bay-Latvia have been used. The Object-oriented Simple Linear Clustering method has been utilized to extract shoreline of Riga Bay. Bend and Douglas-Peucker methods have been used to simplify the extracted shoreline to test the effect of both methods. Photogrammetrically digitized shoreline has been taken as reference data to compare obtained results. The accuracy assessment has been realised by Digital Shoreline Analysis tool. As a result, the achieved shoreline by the Bend method has been found closer to the extracted shoreline with Simple Linear Clustering method.

Simple method for the extraction and reversed-phase high-performance liquid chromatographic analysis of carotenoid pigments from red yeasts (Basidiomycota, Fungi).

PubMed

Weber, Roland W S; Anke, Heidrun; Davoli, Paolo

2007-03-23

A simple method for the extraction of carotenoid pigments from frozen wet cells of red yeasts (Basidiomycota) and their analysis by reversed-phase HPLC using a C(18) column and a water/acetone solvent system is described. Typical red yeast carotenoids belonging to an oxidative series from the monocyclic gamma-carotene to 2-hydroxytorularhodin and from the bicyclic beta-carotene to astaxanthin were separated. Pigment identity was confirmed by LC-atmospheric pressure chemical ionisation (APCI) mass spectrometry using similar chromatographic conditions.

Optical character recognition with feature extraction and associative memory matrix

NASA Astrophysics Data System (ADS)

Sasaki, Osami; Shibahara, Akihito; Suzuki, Takamasa

1998-06-01

A method is proposed in which handwritten characters are recognized using feature extraction and an associative memory matrix. In feature extraction, simple processes such as shifting and superimposing patterns are executed. A memory matrix is generated with singular value decomposition and by modifying small singular values. The method is optically implemented with two liquid crystal displays. Experimental results for the recognition of 25 handwritten alphabet characters clearly shows the effectiveness of the method.

Simple and efficient method for region of interest value extraction from picture archiving and communication system viewer with optical character recognition software and macro program.

PubMed

Lee, Young Han; Park, Eun Hae; Suh, Jin-Suck

2015-01-01

The objectives are: 1) to introduce a simple and efficient method for extracting region of interest (ROI) values from a Picture Archiving and Communication System (PACS) viewer using optical character recognition (OCR) software and a macro program, and 2) to evaluate the accuracy of this method with a PACS workstation. This module was designed to extract the ROI values on the images of the PACS, and created as a development tool by using open-source OCR software and an open-source macro program. The principal processes are as follows: (1) capture a region of the ROI values as a graphic file for OCR, (2) recognize the text from the captured image by OCR software, (3) perform error-correction, (4) extract the values including area, average, standard deviation, max, and min values from the text, (5) reformat the values into temporary strings with tabs, and (6) paste the temporary strings into the spreadsheet. This principal process was repeated for the number of ROIs. The accuracy of this module was evaluated on 1040 recognitions from 280 randomly selected ROIs of the magnetic resonance images. The input times of ROIs were compared between conventional manual method and this extraction module-assisted input method. The module for extracting ROI values operated successfully using the OCR and macro programs. The values of the area, average, standard deviation, maximum, and minimum could be recognized and error-corrected with AutoHotkey-coded module. The average input times using the conventional method and the proposed module-assisted method were 34.97 seconds and 7.87 seconds, respectively. A simple and efficient method for ROI value extraction was developed with open-source OCR and a macro program. Accurate inputs of various numbers from ROIs can be extracted with this module. The proposed module could be applied to the next generation of PACS or existing PACS that have not yet been upgraded. Copyright © 2015 AUR. Published by Elsevier Inc. All rights reserved.

Stroke-model-based character extraction from gray-level document images.

PubMed

Ye, X; Cheriet, M; Suen, C Y

2001-01-01

Global gray-level thresholding techniques such as Otsu's method, and local gray-level thresholding techniques such as edge-based segmentation or the adaptive thresholding method are powerful in extracting character objects from simple or slowly varying backgrounds. However, they are found to be insufficient when the backgrounds include sharply varying contours or fonts in different sizes. A stroke-model is proposed to depict the local features of character objects as double-edges in a predefined size. This model enables us to detect thin connected components selectively, while ignoring relatively large backgrounds that appear complex. Meanwhile, since the stroke width restriction is fully factored in, the proposed technique can be used to extract characters in predefined font sizes. To process large volumes of documents efficiently, a hybrid method is proposed for character extraction from various backgrounds. Using the measurement of class separability to differentiate images with simple backgrounds from those with complex backgrounds, the hybrid method can process documents with different backgrounds by applying the appropriate methods. Experiments on extracting handwriting from a check image, as well as machine-printed characters from scene images demonstrate the effectiveness of the proposed model.

Lipid Extraction and Cholesterol Quantification: A Simple Protocol

ERIC Educational Resources Information Center

Barreto, M. Carmo

2005-01-01

Enzymatic methods are used to measure cholesterol levels but a simple and inexpensive method is described, which is particularly important when one has repeated lab sessions during the week. It can be carried out on the organic phase containing the lipids, without evaporating the solvent, yielding quick results.

Measurement of fumonisins in corn with a fiber optic fluoroimmunosensor

NASA Astrophysics Data System (ADS)

Thompson, Vicki S.; Maragos, Chris M.

1997-05-01

A fiber-optic immunosensor was used to determine concentrations of the mycotoxin fumonisin B1(FB1) in both spiked and naturally contaminated corn samples. Samples were extracted with a mixture of methanol/water. Two methods were used to prepare the methanolic corn extracts before introduction to the immunosensor: (1) simple dilution of the methanolic corn extract; or (2) affinity column cleanup. The sensor displayed an IC50 of 70 ng FB1/mL when toxin was introduced in phosphate buffered saline. Simple dilution of methanolic corn extracts yielded an assay with an IC50 equivalent to 25 (mu) gFB1/g corn and a limit of detection of 3.2 (mu) g/g corn, while affinity cleanup of corn extracts yielded an assay with an IC50 of 5 (mu) gFB1/g corn and a limit of detection of 0.4 (mu) gFB1/g corn. The difference in sensitivity between the two cleanup techniques was due to concentration of fumonisins obtained from the affinity cleanup procedure. Naturally contaminated corn samples were also analyzed after either simple dilution or affinity column cleanup. For comparison the naturally contaminated corn samples were analyzed with an HPLC method after isolation of the fumonisins with strong anion exchange (SAX) solid phase extraction cartridges. The SAX/HPLC method and the immunosensor method agreed well except when large amounts of other fumonisins (i.e. fumonisin B2) were present. This was due in part to the cross-reactivity of the monoclonal antibody with other fumonisins. The immunosensor has the potential to screen individual corn samples for fumonisins within six minutes, and is among the fastest of the currently available FB1 detection methods.

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.

Bio-based extraction and stabilization of anthocyanins.

PubMed

Roy, Anirban; Mukherjee, Rudra Palash; Howard, Luke; Beitle, Robert

2016-05-01

This work reports a novel method of recovering anthocyanin compounds from highly-pigmented grapes via a fermentation based approach. It was hypothesized that batch growth of Zymomonas mobilis on simple medium would produce both ethanol and enzymes/biomass-acting materials, the combination of which will provide a superior extraction when compared to simple alcohol extraction. To examine this hypothesis, Z. mobilis was fermented in a batch consisting of mashed Vitis vinifera and glucose, and the recovered anthocyanin pool was compared to that recovered via extraction with ethanol. Data indicated higher amounts of anthocyanins were recovered when compared to simple solvent addition. Additionally, the percent polymeric form of the anthocyanins could be manipulated by the level of aeration maintained in the fermentation. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:601-605, 2016. © 2016 American Institute of Chemical Engineers.

Correction of Atmospheric Haze in RESOURCESAT-1 LISS-4 MX Data for Urban Analysis: AN Improved Dark Object Subtraction Approach

NASA Astrophysics Data System (ADS)

Mustak, S.

2013-09-01

The correction of atmospheric effects is very essential because visible bands of shorter wavelength are highly affected by atmospheric scattering especially of Rayleigh scattering. The objectives of the paper is to find out the haze values present in the all spectral bands and to correct the haze values for urban analysis. In this paper, Improved Dark Object Subtraction method of P. Chavez (1988) is applied for the correction of atmospheric haze in the Resoucesat-1 LISS-4 multispectral satellite image. Dark object Subtraction is a very simple image-based method of atmospheric haze which assumes that there are at least a few pixels within an image which should be black (% reflectance) and such black reflectance termed as dark object which are clear water body and shadows whose DN values zero (0) or Close to zero in the image. Simple Dark Object Subtraction method is a first order atmospheric correction but Improved Dark Object Subtraction method which tends to correct the Haze in terms of atmospheric scattering and path radiance based on the power law of relative scattering effect of atmosphere. The haze values extracted using Simple Dark Object Subtraction method for Green band (Band2), Red band (Band3) and NIR band (band4) are 40, 34 and 18 but the haze values extracted using Improved Dark Object Subtraction method are 40, 18.02 and 11.80 for aforesaid bands. Here it is concluded that the haze values extracted by Improved Dark Object Subtraction method provides more realistic results than Simple Dark Object Subtraction method.

Masquerade Detection Using a Taxonomy-Based Multinomial Modeling Approach in UNIX Systems

DTIC Science & Technology

2008-08-25

primarily the modeling of statistical features , such as the frequency of events, the duration of events, the co- occurrence of multiple events...are identified, we can extract features representing such behavior while auditing the user’s behavior. Figure1: Taxonomy of Linux and Unix...achieved when the features are extracted just from simple commands. Method Hit Rate False Positive Rate ocSVM using simple cmds (freq.-based

A simple method for determination of carmine in food samples based on cloud point extraction and spectrophotometric detection.

PubMed

Heydari, Rouhollah; Hosseini, Mohammad; Zarabi, Sanaz

2015-01-01

In this paper, a simple and cost effective method was developed for extraction and pre-concentration of carmine in food samples by using cloud point extraction (CPE) prior to its spectrophotometric determination. Carmine was extracted from aqueous solution using Triton X-100 as extracting solvent. The effects of main parameters such as solution pH, surfactant and salt concentrations, incubation time and temperature were investigated and optimized. Calibration graph was linear in the range of 0.04-5.0 μg mL(-1) of carmine in the initial solution with regression coefficient of 0.9995. The limit of detection (LOD) and limit of quantification were 0.012 and 0.04 μg mL(-1), respectively. Relative standard deviation (RSD) at low concentration level (0.05 μg mL(-1)) of carmine was 4.8% (n=7). Recovery values in different concentration levels were in the range of 93.7-105.8%. The obtained results demonstrate the proposed method can be applied satisfactory to determine the carmine in food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantification of Sesquiterpene Lactones in Asteraceae Plant Extracts: Evaluation of their Allergenic Potential

PubMed Central

Salapovic, Helena; Geier, Johannes; Reznicek, Gottfried

2013-01-01

Sesquiterpene lactones (SLs), mainly those with an activated exocyclic methylene group, are important allergens in Asteraceae (Compositae) plants. As a screening tool, the Compositae mix, consisting of five Asteraceae plant extracts with allergenic potential (feverfew, tansy, arnica, yarrow, and German chamomile) is part of several national patch test baseline series. However, the SL content of the Compositae mix may vary due to the source material. Therefore, a simple spectrophotometric method for the quantitative measurement of SLs with the α-methylene-γ-butyrolactone moiety was developed, giving the percentage of allergenic compounds in plant extracts. The method has been validated and five Asteraceae extracts, namely feverfew (Tanacetum parthenium L.), tansy (Tanacetum vulgare L.), arnica (Arnica montana L.), yarrow (Achillea millefolium L.), and German chamomile (Chamomilla recutita L. Rauschert) that have been used in routine patch test screening were evaluated. A good correlation could be found between the results obtained using the proposed spectrophotometric method and the corresponding clinical results. Thus, the introduced method is a valuable tool for evaluating the allergenic potential and for the simple and efficient quality control of plant extracts with allergenic potential. PMID:24106675

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

PubMed

Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

2018-05-01

A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid methods for extraction and concentration of poliovirus from oyster tissues.

PubMed

Richards, G P; Goldmintz, D; Green, D L; Babinchak, J A

1982-12-01

A procedure is discussed for the extraction of poliovirus from oyster meats by modification of several enterovirus extraction techniques. The modified method uses meat extract and Cat-Floc, a polycationic electrolyte, for virus extraction and concentration. Virus recovery from inoculated oyster homogenates is 93-120%. Adsorption of viruses to oyster proteins by acidification of homogenates does not affect virus recovery. Elution of viruses from oyster proteins appears more efficient at pH 9.5 than at pH 8.0. This technique is relatively simple, economical and requires only 2.5 h to complete the combined extraction and concentration procedure.

Ultra-Trace Analysis of Nine Macrolides, including Tulathromycin A (Draxxin), in Edible Animal Tissues with Mini-Column Liquid Chromatography Tandem Mass Spectrometry

USDA-ARS?s Scientific Manuscript database

Analysis of 9 macrolides is presented, including tulathromycin A (Draxxin), in beef, poultry and pork muscle with a simple multi-residue extraction and analysis method using high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry. The extraction method inv...

SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

EPA Science Inventory

A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

PRELIMINARY COMPARATIVE STUDY OF METHODS TO EXTRACT VIRUS FROM RAW AND PROCESSED SEWAGE SLUDGES

EPA Science Inventory

Two simple virus extraction techniques were compared to an EPA standard method for detection of human enteric viruses in raw sewage sludge and class A biosolids. The techniques were used to detect both indigenous and seeded virus from a plant that distributes class A material pr...

Optimisation of a simple and reliable method based on headspace solid-phase microextraction for the determination of volatile phenols in beer.

PubMed

Pizarro, C; Pérez-del-Notario, N; González-Sáiz, J M

2010-09-24

A simple, accurate and sensitive method based on headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the analysis of 4-ethylguaiacol, 4-ethylphenol, 4-vinylguaiacol and 4-vinylphenol in beer. The effect of the presence of CO2 in the sample on the extraction of analytes was examined. The influence on extraction efficiency of different fibre coatings, of salt addition and stirring was also evaluated. Divinylbenzene/carboxen/polydimethylsiloxane was selected as extraction fibre and was used to evaluate the influence of exposure time, extraction temperature and sample volume/total volume ratio (Vs/Vt) by means of a central composite design (CCD). The optimal conditions identified were 80 degrees C for extraction temperature, 55 min for extraction time and 6 mL of beer (Vs/Vt 0.30). Under optimal conditions, the proposed method showed satisfactory linearity (correlation coefficients between 0.993 and 0.999), precision (between 6.3% and 9.7%) and detection limits (lower than those previously reported for volatile phenols in beers). The method was applied successfully to the analysis of beer samples. To our knowledge, this is the first time that a HS-SPME based method has been developed to determine simultaneously these four volatile phenols in beers. Copyright 2010 Elsevier B.V. All rights reserved.

New method for the extraction of bulk channel mobility and flat-band voltage in junctionless transistors

NASA Astrophysics Data System (ADS)

Jeon, Dae-Young; Park, So Jeong; Mouis, Mireille; Barraud, Sylvain; Kim, Gyu-Tae; Ghibaudo, Gérard

2013-11-01

A new and simple method for the extraction of electrical parameters in junctionless transistors (JLTs) is presented. The bulk channel mobility (μbulk) and flat-band voltage (Vfb) were successfully extracted from the new method, based on a linear dependence between the inverse of transconductance squared (1/gm2) vs gate voltage in the partially depleted operation regime (Vth < Vg < Vfb). The validity of the new method is also proved by 2D numerical simulation and newly defined Maserjian's-like function for gm of JLT devices.

Light extraction from organic light-emitting diodes for lighting applications by sand-blasting substrates.

PubMed

Chen, Shuming; Kwok, Hoi Sing

2010-01-04

Light extraction from organic light-emitting diodes (OLEDs) by scattering the light is one of the effective methods for large-area lighting applications. In this paper, we present a very simple and cost-effective method to rough the substrates and hence to scatter the light. By simply sand-blasting the edges and back-side surface of the glass substrates, a 20% improvement of forward efficiency has been demonstrated. Moreover, due to scattering effect, a constant color over all viewing angles and uniform light pattern with Lambertian distribution has been obtained. This simple and cost-effective method may be suitable for mass production of large-area OLEDs for lighting applications.

Olea europaea L. leaf extract and derivatives: antioxidant properties.

PubMed

Briante, Raffaella; Patumi, Maurizio; Terenziani, Stefano; Bismuto, Ettore; Febbraio, Ferdinando; Nucci, Roberto

2002-08-14

This paper reports a very simple and fast method to collect eluates with high amounts of hydroxytyrosol, biotransforming Olea europaea L. leaf extract by a thermophilic beta-glycosidase immobilized on chitosan. Some phenolic compounds in the leaf tissue and in the eluates obtained by biotransformation are identified. To propose the eluates as natural substances from a vegetal source, their antioxidant properties have been compared with those of the leaf extract from which they are originated. The eluates possess a higher concentration of simple phenols, characterized by a stronger antioxidant capacity, than those available in extra virgin olive oils and in many tablets of olive leaf extracts, commercially found as dietetic products and food integrators.

Simple saponification method for the quantitative determination of carotenoids in green vegetables.

PubMed

Larsen, Erik; Christensen, Lars P

2005-08-24

A simple, reliable, and gentle saponification method for the quantitative determination of carotenoids in green vegetables was developed. The method involves an extraction procedure with acetone and the selective removal of the chlorophylls and esterified fatty acids from the organic phase using a strongly basic resin (Ambersep 900 OH). Extracts from common green vegetables (beans, broccoli, green bell pepper, chive, lettuce, parsley, peas, and spinach) were analyzed by high-performance liquid chromatography (HPLC) for their content of major carotenoids before and after action of Ambersep 900 OH. The mean recovery percentages for most carotenoids [(all-E)-violaxanthin, (all-E)-lutein epoxide, (all-E)-lutein, neolutein A, and (all-E)-beta-carotene] after saponification of the vegetable extracts with Ambersep 900 OH were close to 100% (99-104%), while the mean recovery percentages of (9'Z)-neoxanthin increased to 119% and that of (all-E)-neoxanthin and neolutein B decreased to 90% and 72%, respectively.

Image segmentation-based robust feature extraction for color image watermarking

NASA Astrophysics Data System (ADS)

Li, Mianjie; Deng, Zeyu; Yuan, Xiaochen

2018-04-01

This paper proposes a local digital image watermarking method based on Robust Feature Extraction. The segmentation is achieved by Simple Linear Iterative Clustering (SLIC) based on which an Image Segmentation-based Robust Feature Extraction (ISRFE) method is proposed for feature extraction. Our method can adaptively extract feature regions from the blocks segmented by SLIC. This novel method can extract the most robust feature region in every segmented image. Each feature region is decomposed into low-frequency domain and high-frequency domain by Discrete Cosine Transform (DCT). Watermark images are then embedded into the coefficients in the low-frequency domain. The Distortion-Compensated Dither Modulation (DC-DM) algorithm is chosen as the quantization method for embedding. The experimental results indicate that the method has good performance under various attacks. Furthermore, the proposed method can obtain a trade-off between high robustness and good image quality.

SIMPLE SAMPLE CLEAN UP PROCEDURE AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE ANALYSIS OF CYANURIC ACID IN HUMAN URINE

EPA Science Inventory

Cyanuric acide (CA) is widely used as a chlorine stabilizer in outdoor pools. No simple method exists for CA measurement in the urine of exposed swimmers. The high hydrophilicity of CA makes usage of solid phase sorbents to extract it from urine nearly impossible because of samp...

Fast, safe, and reliable methods for extraction of major inorganic cations from small quantities of woody plant tissues

Treesearch

Rakesh Minocha; Walter C. Shortle

1993-01-01

Two simple and fast methods for the extraction of major inorganic cations (Ca, Mg, Mn, K) from small quantities of stemwood and needles of woody plants were developed. A 3.2- or 6.4-mm cobalt drill bit was used to shave samples from disks and increment cores of stemwood. For ion extraction, wood (ground or shavings) or needles were either homogenzied using a Tekmar...

Optimizing Standard Sequential Extraction Protocol With Lake And Ocean Sediments

EPA Science Inventory

The environmental mobility/availability behavior of radionuclides in soils and sediments depends on their speciation. Experiments have been carried out to develop a simple but robust radionuclide sequential extraction method for identification of radionuclide partitioning in sed...

Field method for the determination of hexavalent chromium by ultrasonication and strong anion-exchange solid-phase extraction.

PubMed

Wang, J; Ashley, K; Marlow, D; England, E C; Carlton, G

1999-03-01

A simple, fast, sensitive, and economical field method was developed and evaluated for the determination of hexavalent chromium (CrVI) in environmental and workplace air samples. By means of ultrasonic extraction in combination with a strong anion-exchange solid-phase extraction (SAE-SPE) technique, the filtration, isolation, and determination of CrVI in the presence of trivalent chromium (CrIII) and potential interferents was achieved. The method entails (1) ultrasonication in basic ammonium buffer solution to extract CrVI from environmental matrixes; (2) SAE-SPE to separate CrVI from CrIII and interferences; (3) elution/acidification of the eluate; (4) complexation of chromium with 1,5-diphenylcarbazide; and (5) spectrophotometric determination of the colored chromium-diphenylcarbazone complex. Several critical parameters were optimized in order to effect the extraction of both soluble (K2CrO4) and insoluble (PbCrO4) forms of CrVI without inducing CrIII oxidation or CrVI reduction. The method allowed for the dissolution and purification of CrVI from environmental and workplace air sample matrixes for up to 24 samples simultaneously in less than 90 min (including ultrasonication). The results demonstrated that the method was simple, fast, quantitative, and sufficiently sensitive for the determination of occupational exposures of CrVI. The method is applicable for on-site monitoring of CrVI in environmental and industrial hygiene samples.

Sorptive thin film microextraction followed by direct solid state spectrofluorimetry: A simple, rapid and sensitive method for determination of carvedilol in human plasma.

PubMed

Karimi, Shima; Talebpour, Zahra; Adib, Noushin

2016-06-14

A poly acrylate-ethylene glycol (PA-EG) thin film is introduced for the first time as a novel polar sorbent for sorptive extraction method coupled directly to solid-state spectrofluorimetry without the necessity of a desorption step. The structure, polarity, fluorescence property and extraction performance of the developed thin film were investigated systematically. Carvedilol was used as the model analyte to evaluate the proposed method. The entire procedure involved one-step extraction of carvedilol from plasma using PA-EG thin film sorptive phase without protein precipitation. Extraction variables were studied in order to establish the best experimental conditions. Optimum extraction conditions were the followings: stirring speed of 1000 rpm, pH of 6.8, extraction temperature of 60 °C, and extraction time of 60 min. Under optimal conditions, extraction of carvedilol was carried out in spiked human plasma; and the linear range of calibration curve was 15-300 ng mL(-1) with regression coefficient of 0.998. Limit of detection (LOD) for the method was 4.5 ng mL(-1). The intra- and inter-day accuracy and precision of the proposed method were evaluated in plasma sample spiked with three concentration levels of carvedilol; yielding a recovery of 91-112% and relative standard deviation of less than 8%, respectively. The established procedure was successfully applied for quantification of carvedilol in plasma sample of a volunteer patient. The developed PA-EG thin film sorptive phase followed by solid-state spectrofluorimetric method provides a simple, rapid and sensitive approach for the analysis of carvedilol in human plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of a sensitive high-performance liquid chromatographic method with simple extraction for simultaneous determination of huperzine A and huperzine B in the species containing lycopodium alkaloids.

PubMed

Zhang, Yanqing; Xie, Junbo; Chen, Wen-Qian; Zhou, Tian-Yan; Lu, Wei

2009-01-01

A sensitive HPLC method with simple extraction was developed for simultaneous determination of huperzine A (HupA) and huperzine B (HupB) in Huperzia serrata, H. crispata, H. miyoshiana, and Lycopodiastrum casuarinoides. In order to avoid conventional multiple-step and time-consuming sample preparation methods, direct reflux extraction with alkaline chloroform was adopted. The quantitative determination was conducted by reversed-phase HPLC with a photodiode array detector set at 308 nm. Separation was performed on a Luna C18 column (250 x 4.6 mm id, 5 microm) with methanol-0.2% aqueous acetic acid (18 + 82, v/v) mobile phase. The method was validated for accuracy, reproducibility, precision, and limits of detection and quantification. Quantification of the two active compounds in the samples was performed by this newly developed method, and the content of HupA and HupB varied substantially among four different species. The satisfactory results indicated that the developed method can readily be utilized for quality control of the species of Huperziaceae and Lycopodiaceae containing the two compounds.

Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples.

PubMed

Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Zhu, Gang-Tian; Yuan, Bi-Feng; Feng, Yu-Qi

2016-01-01

In this study, we proposed a method to fabricate magnetic carbon nitride (CN) nanosheets by simple physical blending. Low-cost CN nanosheets prepared by urea possessed a highly π-conjugated structure; therefore the obtained composites were employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oil samples. Moreover, sample pre-treatment time could be carried out within 10 min. Thus, a simple and cheap method for the analysis of PAHs in edible oil samples was established by coupling magnetic CN nanosheets-based MSPE with gas chromatography-mass spectrometry (GC/MS) analysis. Limits of quantitation (LOQs) for eight PAHs ranged from 0.4 to 0.9 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 15.0%. The recoveries of PAHs for spiked soybean oil samples ranged from 91.0% to 124.1%, with RSDs of less than 10.2%. Taken together, the proposed method offers a simple and cost-effective option for the convenient analysis of PAHs in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

A Simple Method for Nucleon-Nucleon Cross Sections in a Nucleus

NASA Technical Reports Server (NTRS)

Tripathi, R. K.; Cucinotta, Francis A.; Wilson, John W.

1999-01-01

A simple reliable formalism is presented for obtaining nucleon-nucleon cross sections within a nucleus in nuclear collisions for a given projectile and target nucleus combination at a given energy for use in transport, Monte Carlo, and other calculations. The method relies on extraction of these values from experiments and has been tested and found to give excellent results.

Easy, fast and environmental friendly method for the simultaneous extraction of the 16 EPA PAHs using magnetic molecular imprinted polymers (mag-MIPs).

PubMed

Villar-Navarro, Mercedes; Martín-Valero, María Jesús; Fernández-Torres, Rut Maria; Callejón-Mochón, Manuel; Bello-López, Miguel Ángel

2017-02-15

An easy and environmental friendly method, based on the use of magnetic molecular imprinted polymers (mag-MIPs) is proposed for the simultaneous extraction of the 16 U.S. EPA polycyclic aromatic hydrocarbons (PAHs) priority pollutants. The mag-MIPs based extraction protocol is simple, more sensitive and low organic solvent consuming compared to official methods and also adequate for those PAHs more retained in the particulate matter. The new proposed extraction method followed by HPLC determination has been validated and applied to different types of water samples: tap water, river water, lake water and mineral water. Copyright © 2017 Elsevier B.V. All rights reserved.

[Rapid detection of caffeine in blood by freeze-out extraction].

PubMed

Bekhterev, V N; Gavrilova, S N; Kozina, E P; Maslakov, I V

2010-01-01

A new method for the detection of caffeine in blood has been proposed based on the combination of extraction and freezing-out to eliminate the influence of sample matrix. Metrological characteristics of the method are presented. Selectivity of detection is achieved by optimal conditions of analysis by high performance liquid chromatography. The method is technically simple and cost-efficient, it ensures rapid performance of the studies.

A simple, rapid atmospheric pressure chemical ionization liquid chromatography tandem mass spectrometry method for the determination of 25-hydroxyvitamin D2 and D3.

PubMed

Garg, Uttam; Munar, Ada; Frazee, Clinton; Scott, David

2012-09-01

Vitamin D plays a vital role not only in bone health but also in pathophysiology of many other body functions. In recent years, there has been significant increase in testing of 25-hydroxyvitamin D (25-OH vitamin D), a marker of vitamin D deficiency. The most commonly used methods for the measurement of 25-OH vitamin D are immunoassays and liquid chromatography tandem mass spectrometry (LC-MS-MS). Since immunoassays suffer from inaccuracies and interferences, LC-MS-MS is a preferred method. In LC-MS-MS methods, 25-OH vitamin D is extracted from serum or plasma by solid-phase or liquid-phase extraction. Because these extraction methods are time consuming, we developed an easy method that uses simple protein precipitation followed by injection of the supernatant to LC-MS-MS. Several mass-to-charge (m/z) ratio transitions, including commonly used transitions based on water loss, were evaluated and several tube types were tested. The optimal transitions for 25-OH vitamin D2 and D3 were 395.5 > 269.5 and 383.4 > 257.3, respectively. The reportable range of the method was 1-100 ng/mL, and repeatability (within-run) and within-laboratory imprecision were <4% and <6%, respectively. The method agreed well with the solid-phase extraction methods. © 2012 Wiley Periodicals, Inc.

Molecularly imprinted microspheres synthesized by a simple, fast, and universal suspension polymerization for selective extraction of the topical anesthetic benzocaine in human serum and fish tissues.

PubMed

Sun, Hui; Lai, Jia-Ping; Chen, Fang; Zhu, De-Rong

2015-02-01

A simple, fast, and universal suspension polymerization method was used to synthesize the molecularly imprinted microspheres (MIMs) for the topical anesthetic benzocaine (BZC). The desired diameter (10-20 μm) and uniform morphology of the MIMs were obtained easily by changing one or more of the synthesis conditions, including type and amount of surfactant, stirring rate, and ratio of organic to water phase. The MIMs obtained were used as a molecular-imprinting solid-phase-extraction (MISPE) material for extraction of BZC in human serum and fish tissues. The MISPE results revealed that the BZC in these biosamples could be enriched effectively after the MISPE operation. The recoveries of BZC on MIMs cartridges were higher than 90% (n = 3). Finally, an MISPE-HPLC method with UV detection was developed for highly selective extraction and fast detection of trace BZC in human serum and fish tissues. The developed method could also be used for the enrichment and detection of BZC in other complex biosamples.

Highly Simple Deep Eutectic Solvent Extraction of Manganese in Vegetable Samples Prior to Its ICP-OES Analysis.

PubMed

Bağda, Esra; Altundağ, Hüseyin; Soylak, Mustafa

2017-10-01

In the present work, simple and sensitive extraction methods for selective determination of manganese have been successfully developed. The methods were based on solubilization of manganese in deep eutectic solvent medium. Three deep eutectic solvents with choline chloride (vitamin B4) and tartaric/oxalic/citric acids have been prepared. Extraction parameters were optimized with using standard reference material (1573a tomato leaves). The quantitative recovery values were obtained with 1.25 g/L sample to deep eutectic solvent (DES) volume, at 95 °C for 2 h. The limit of detection was found as 0.50, 0.34, and 1.23 μg/L for DES/tartaric, DES/oxalic, and DES/citric acid, respectively. At optimum conditions, the analytical signal was linear for the range of 10-3000 μg/L for all studied DESs with the correlation coefficient >0.99. The extraction methods were applied to different real samples such as basil herb, spinach, dill, and cucumber barks. The known amount of manganese was spiked to samples, and good recovery results were obtained.

An Improved Method for the Extraction and Thin-Layer Chromatography of Chlorophyll A and B from Spinach

ERIC Educational Resources Information Center

Quach, Hao T.; Steeper, Robert L.; Griffin, William G.

2004-01-01

A simple and fast method, which resolves chlorophyll a and b from spinach leaves on analytical plates while minimizing the appearance of chlorophyll degradation products is shown. An improved mobile phase for the Thin-layer chromatographic analysis of spinach extract that allows for the complete resolution of the common plant pigments found in…

Chemical Composition Analysis of Extracts from Ficus Hirta Using Supercritical Fluid

NASA Astrophysics Data System (ADS)

Deng, S. B.; Chen, J. P.; Chen, Y. Z.; Yu, C. Q.; Yang, Y.; Wu, S. H.; Chen, C. Z.

2018-05-01

Ficus hirta was extracted by supercritical carbon dioxide. The volatile chemical components of extracts were analyzed using gas chromatography-mass spectrometry (GC-MS). The percentage of products extracted by Supercritical Fluid Extraction(SFE) was 2.5%. Nineteen volatile compounds were identified. The main volatile components were Elemicin, Psoralen, Palmitic acid, Bergapten, α-Linolenic acid, Medicarpin, Retinoic Acid, Maackiain, and Squalene. The method is simple and quick, and can be used for the preliminary analysis of chemical constituents of supercritical extracts of Ficus hirta.

Multiclass mycotoxin analysis in edible oils using a simple solvent extraction method and liquid chromatography with tandem mass spectrometry.

PubMed

Eom, Taeyong; Cho, Hyun-Deok; Kim, Junghyun; Park, Mihee; An, Jinyoung; Kim, Moosung; Kim, Sheen-Hee; Han, Sang Beom

2017-11-01

A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B 1 , B 2 , G 1 and G 2 ; fumonisins B 1 , B 2 and B 3 ; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.

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.

Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

PubMed

Sobhi, Hamid Reza; Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali

2017-03-03

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL -1 and 50-1000ngL -1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

PubMed

Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

2017-10-06

Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

Application of FTA technology to extraction of sperm DNA from mixed body fluids containing semen.

PubMed

Fujita, Yoshihiko; Kubo, Shin-ichi

2006-01-01

FTA technology is a novel method designed to simplify the collection, shipment, archiving and purification of nucleic acids from a wide variety of biological sources. In this study, we report a rapid and simple method of extracting DNA from sperm when body fluids mixed with semen were collected using FTA cards. After proteinase K digestion of the sperm and body fluid mixture, the washed pellet suspension as the sperm fraction and the concentrated supernatant as the epithelial cell fraction were respectively applied to FTA cards containing DTT. The FTA cards were dried, then directly added to a polymerase chain reaction (PCR) mix and processed by PCR. The time required from separation of the mixed fluid into sperm and epithelial origin DNA extractions was only about 2.5-3h. Furthermore, the procedure was extremely simple. It is considered that our designed DNA extraction procedure using an FTA card is available for application to routine work.

Simultaneous Determination and Pharmacokinetic Comparisons of Multi-Ingredients after Oral Administration of Radix Salviae Miltiorrhizae Extract, Hawthorn Extract, and a Combination of Both Extracts to Rats

PubMed Central

Liu, Yu-Qiang; Cai, Qian; Liu, Chang; Bao, Feng-Wei; Zhang, Zhen-Qiu

2014-01-01

A simple and sensitive HPLC method was developed for simultaneous determination of danshensu (DSS), rosmarinic acid (RA), lithospermic acid (LA), salvianolic acid B (SAB), and hyperoside (HP) in rat plasma. This method validated was successfully applied to the pharmacokinetic study of the main active ingredients after oral administration of Radix Salviae Miltiorrhizae extract (SME), hawthorn extract (HTE), and a combination of both extracts (2.5 : 1) to rats. The results indicated that there have been great differences in pharmacokinetics between a single extract and a combination of both extracts. A combination of both extracts can enhance their bioavailabilities and delay the elimination of SAB and DSS in rats. PMID:24660090

An ultrasensitive chemiluminescence immunoassay of chloramphenicol based on gold nanoparticles and magnetic beads.

PubMed

Tao, Xiaoqi; Jiang, Haiyang; Yu, Xuezhi; Zhu, Jinghui; Wang, Xia; Wang, Zhanhui; Niu, Lanlan; Wu, Xiaoping; Shen, Jianzhong

2013-05-01

A competitive, direct, chemiluminescent immunoassay based on a magnetic beads (MBs) separation and gold nanoparticles (AuNPs) labelling technique to detect chloramphenicol (CAP) has been developed. Horseradish peroxidase (HRP)-labelled anti-CAP monoclonal antibody conjugated with AuNPs and antigen-immobilized MBs were prepared. After optimization parameters of immunocomplex MBs, the IC50 values of chemiluminescence magnetic nanoparticles immunoassay (CL-MBs-nano-immunoassay) were 0.017 µg L(-1) for extract method I and 0.17 µg L(-1) for extract method II. The immunoassay with two extract methods was applied to detect CAP in milk. Comparison of these two extract methods showed that extract method I was advantageous in better sensitivity, in which the sensitivity was 10 times compared to that of extract method II, while extract method II was superior in simple operation, suitable for high throughout screen. The recoveries were 86.7-98.0% (extract method I) and 80.0-103.0% (extract method II), and the coefficients of variation (CVs) were all <15%. The satisfactory recovery with both extract methods and high correlation with traditional ELISA kit in milk system confirmed that the immunomagnetic assay based on AuNPs exhibited promising potential in rapid field screening for trace CAP analysis. Copyright © 2013 John Wiley & Sons, Ltd.

In-tube electro-membrane extraction with a sub-microliter organic solvent consumption as an efficient technique for synthetic food dyes determination in foodstuff samples.

PubMed

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Asghari, Alireza; Abdossalami asl, Yousef

2015-09-04

A simple and efficient extraction technique with a sub-microliter organic solvent consumption termed as in-tube electro-membrane extraction (IEME) is introduced. This method is based upon the electro-kinetic migration of ionized compounds by the application of an electrical potential difference. For this purpose, a thin polypropylene (PP) sheet placed inside a tube acts as a support for the membrane solvent, and 30μL of an aqueous acceptor solution is separated by this solvent from 1.2mL of an aqueous donor solution. This method yielded high extraction recoveries (63-81%), and the consumption of the organic solvent used was only 0.5μL. By performing this method, the purification is high, and the utilization of the organic solvent, used as a mediator, is very simple and repeatable. The proposed method was evaluated by extraction of four synthetic food dyes (Amaranth, Ponceau 4R, Allura Red, and Carmoisine) as the model analytes. Optimization of variables affecting the method was carried out in order to achieve the best extraction efficiency. These variables were the type of membrane solvent, applied extraction voltage, extraction time, pH range, and concentration of salt added. Under the optimized conditions, IEME-HPLC-UV provided a good linearity in the range of 1.00-800ngmL(-1), low limits of detection (0.3-1ngmL(-1)), and good extraction repeatabilities (RSDs below 5.2%, n=5). It seems that this design is a proper one for the automation of the method. Also the consumption of the organic solvent in a sub-microliter scale, and its simplicity, high efficiency, and high purification can help one getting closer to the objectives of the green chemistry. Copyright © 2015 Elsevier B.V. All rights reserved.

[Isolation and purification of seven catechin compounds from fresh tea leaves by semi-preparative liquid chromatography].

PubMed

Gong, Zhihong; Chen, Si; Gao, Jiangtao; Li, Meihong; Wang, Xiaxia; Lin, Jun; Yu, Xiaomin

2017-11-08

An effective and simple method was established to simultaneously purify seven tea catechins (gallocatechin (GC), epigallocatechin (EGC), catechin (C), epigallocatechin-3- O -gallate (EGCG), epicatechin (EC), epigallocatechin-3- O -(3- O -methyl)-gallate (EGCG3"Me) and epicatechin-3- O -gallate (ECG)) from fresh tea leaves by semi-preparative high performance liquid chromatography (HPLC). Fresh leaves of Tieguanyin tea were successively extracted with methanol and chloroform. Then crude catechins were precipitated from the aqueous fraction of chloroform extraction by adding lead subacetate. Crude catechins were used for the isolation of the seven target catechin compounds by semi-preparative HPLC. Methanol-water and acetonitrile-water were sequentially used as mobile phases. After two rounds of semi-preparative HPLC, all target compounds were achieved with high purities (>90%). The proposed method was tested on two additional tea cultivars and showed similar results. This method demonstrated a simple and efficient strategy based on solvent extraction, ion precipitation and semi-preparative HPLC for the preparation of multiple catechins from tea leaves.

An Isotopic Dilution Experiment Using Liquid Scintillation: A Simple Two-System, Two-Phase Analysis.

ERIC Educational Resources Information Center

Moehs, Peter J.; Levine, Samuel

1982-01-01

A simple isotonic, dilution analysis whose principles apply to methods of more complex radioanalyses is described. Suitable for clinical and instrumental analysis chemistry students, experimental manipulations are kept to a minimum involving only aqueous extraction before counting. Background information, procedures, and results are discussed.…

A RAPID AND SIMPLE PHOSPHOLIPASE A ASSAY,

DTIC Science & Technology

A simple and rapid method for the assay of phospholipase A was developed. As a substrate fresh egg yolk is used which is hydrolyzed by snake venom...phospholipase A at a 10-20 x faster rate than pure lecithin . The released fatty acids, after extraction with appropriate solvents are titrated

[Feature extraction for breast cancer data based on geometric algebra theory and feature selection using differential evolution].

PubMed

Li, Jing; Hong, Wenxue

2014-12-01

The feature extraction and feature selection are the important issues in pattern recognition. Based on the geometric algebra representation of vector, a new feature extraction method using blade coefficient of geometric algebra was proposed in this study. At the same time, an improved differential evolution (DE) feature selection method was proposed to solve the elevated high dimension issue. The simple linear discriminant analysis was used as the classifier. The result of the 10-fold cross-validation (10 CV) classification of public breast cancer biomedical dataset was more than 96% and proved superior to that of the original features and traditional feature extraction method.

Simple high-performance liquid chromatography method for formaldehyde determination in human tissue through derivatization with 2,4-dinitrophenylhydrazine.

PubMed

Yilmaz, Bilal; Asci, Ali; Kucukoglu, Kaan; Albayrak, Mevlut

2016-08-01

A simple high-performance liquid chromatography method has been developed for the determination of formaldehyde in human tissue. FA Formaldehyde was derivatized with 2,4-dinitrophenylhydrazine. It was extracted from human tissue with ethyl acetate by liquid-liquid extraction and analyzed by high-performance liquid chromatography. The calibration curve was linear in the concentration range of 5.0-200 μg/mL. Intra- and interday precision values for formaldehyde in tissue were <6.9%, and accuracy (relative error) was better than 6.5%. The extraction recoveries of formaldehyde from human tissue were between 88 and 98%. The limits of detection and quantification of formaldehyde were 1.5 and 5.0 μg/mL, respectively. Also, this assay was applied to liver samples taken from a biopsy material. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-throughput and selective solid-phase extraction of urinary catecholamines by crown ether-modified resin composite fiber.

PubMed

Chen, LiQin; Wang, Hui; Xu, Zhen; Zhang, QiuYue; Liu, Jia; Shen, Jun; Zhang, WanQi

2018-08-03

In the present study, we developed a simple and high-throughput solid phase extraction (SPE) procedure for selective extraction of catecholamines (CAs) in urine samples. The SPE adsorbents were electrospun composite fibers functionalized with 4-carboxybenzo-18-crown-6 ether modified XAD resin and polystyrene, which were packed into 96-well columns and used for high-throughput selective extraction of CAs in healthy human urine samples. Moreover, the extraction efficiency of packed-fiber SPE (PFSPE) was examined by high performance liquid chromatography coupled with fluorescence detector. The parameters affecting the extraction efficiency and impurity removal efficiency were optimized, and good linearity ranging from 0.5 to 400 ng/mL was obtained with a low limit of detection (LOD, 0.2-0.5 ng/mL) and a good repeatability (2.7%-3.7%, n = 6). The extraction recoveries of three CAs ranged from 70.5% to 119.5%. Furthermore, stable and reliable results obtained by the fluorescence detector were superior to those obtained by the electrochemical detector. Collectively, PFSPE coupled with 96-well columns was a simple, rapid, selective, high-throughput and cost-efficient method, and the proposed method could be applied in clinical chemistry. Copyright © 2018 Elsevier B.V. All rights reserved.

Comparison of the DNA extraction methods for polymerase chain reaction amplification from formalin-fixed and paraffin-embedded tissues.

PubMed

Sato, Y; Sugie, R; Tsuchiya, B; Kameya, T; Natori, M; Mukai, K

2001-12-01

To obtain an adequate quality and quantity of DNA from formalin-fixed and paraffin-embedded tissue, six different DNA extraction methods were compared. Four methods used deparaffinization by xylene followed by proteinase K digestion and phenol-chloroform extraction. The temperature of the different steps was changed to obtain higher yields and improved quality of extracted DNA. The remaining two methods used microwave heating for deparaffinization. The best DNA extraction method consisted of deparaffinization by microwave irradiation, protein digestion with proteinase K at 48 degrees C overnight, and no further purification steps. By this method, the highest DNA yield was obtained and the amplification of a 989-base pair beta-globin gene fragment was achieved. Furthermore, DNA extracted by means of this procedure from five gastric carcinomas was successfully used for single strand conformation polymorphism and direct sequencing assays of the beta-catenin gene. Because the microwave-based DNA extraction method presented here is simple, has a lower contamination risk, and results in a higher yield of DNA compared with the ordinary organic chemical reagent-based extraction method, it is considered applicable to various clinical and basic fields.

Cytotoxic Deoxypodophyllotoxin Can Be Extracted in High Purity from Anthriscus sylvestris Roots by Supercritical Carbon Dioxide.

PubMed

Seegers, Christel L C; Tepper, Pieter G; Setroikromo, Rita; Quax, Wim J

2018-05-01

Deoxypodophyllotoxin is present in the roots of Anthriscus sylvestris . This compound is cytotoxic on its own, but it can also be converted into podophyllotoxin, which is in high demand as a precursor for the important anticancer drugs etoposide and teniposide. In this study, deoxypodophyllotoxin is extracted from A. sylvestris roots by supercritical carbon dioxide extraction. The process is simple and scalable. The supercritical carbon dioxide method extracts 75 - 80% of the total deoxypodophyllotoxin content, which is comparable to a single extraction by traditional Soxhlet. However, less polar components are extracted. The activity of the supercritical carbon dioxide extract containing deoxypodophyllotoxin was assessed by demonstrating that the extract arrests A549 and HeLa cells in the G 2 /M phase of the cell cycle. We conclude that biologically active deoxypodophyllotoxin can be extracted from A. sylvestris by supercritical carbon dioxide extraction. The method is solvent free and more sustainable compared to traditional methods. Georg Thieme Verlag KG Stuttgart · New York.

The Extraction and Partial Purification of Bacterial DNA as a Practical Exercise for GCE Advanced Level Students.

ERIC Educational Resources Information Center

Falconer, A. C.; Hayes, L. J.

1986-01-01

Describes a relatively simple method of extraction and purification of bacterial DNA. This technique permits advanced secondary-level science students to obtain adequate amounts of DNA from very small pellets of bacteria and to observe some of its polymer properties. (ML)

EXTRACTION AND QUANTITATIVE ANALYSIS OF ELEMENTAL SULFUR FROM SULFIDE MINERAL SURFACES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY. (R826189)

EPA Science Inventory

A simple method for the quantitative determination of elemental sulfur on oxidized sulfide minerals is described. Extraction of elemental sulfur in perchloroethylene and subsequent analysis with high-performance liquid chromatography were used to ascertain the total elemental ...

Use of fluorinated polybrominated diphenyl ethers and simplified cleanup for the analysis of polybrominated diphenyl ethers in house dust

EPA Science Inventory

A simple, cost-effective method is described for the analysis of polybrominated diphenyl ethers (PBDEs) in house dust using pressurized fluid extraction, cleanup with modified silica solid phase extraction tubes, and fluorinated internal standards. There are 14 PBDE congeners inc...

A Simple and Fast Extraction Method for the Determination of Multiclass Antibiotics in Eggs Using LC-MS/MS.

PubMed

Wang, Kun; Lin, Kunde; Huang, Xinwen; Chen, Meng

2017-06-21

The purpose of this study was to develop and validate a simple, fast, and specific extraction method for the analysis of 64 antibiotics from nine classes (including sulfonamides, quinolones, tetracyclines, macrolides, lincosamide, nitrofurans, β-lactams, nitromidazoles, and cloramphenicols) in chicken eggs. Briefly, egg samples were simply extracted with a mixture of acetonitrile-water (90:10, v/v) and 0.1 mol·L -1 Na 2 EDTA solution assisted with ultrasonic. The extract was centrifuged, condensed, and directly analyzed on a liquid chromatography coupled to tandem mass spectrometry. Compared with conventional cleanup methods (passing through solid phase extract cartridges), the established method demonstrated comparable efficiencies in eliminating matrix effects and higher or equivalent recoveries for most of the target compounds. Typical validation parameters including specificity, linearity, matrix effect, limits of detection (LODs) and quantification (LOQs), the decision limit, detection capability, trueness, and precision were evaluated. The recoveries of target compounds ranged from 70.8% to 116.1% at three spiking levels (5, 20, and 50 μg·kg -1 ), with relative standard deviations less than 14%. LODs and LOQs were in the ranges of 0.005-2.00 μg·kg -1 and 0.015-6.00 μg·kg -1 for all of the antibiotics, respectively. A total of five antibiotics were successfully detected in 22 commercial eggs from local markets. This work suggests that the method is suitable for the analysis of multiclass antibiotics in eggs.

Analysis of mixtures of fatty acids and fatty alcohols in fermentation broth.

PubMed

Liu, Yilan; Chen, Ting; Yang, Maohua; Wang, Caixia; Huo, Weiyan; Yan, Daojiang; Chen, Jinjin; Zhou, Jiemin; Xing, Jianmin

2014-01-03

Microbial production of fatty acids and fatty alcohols has attracted increasing concerns because of energy crisis and environmental impact of fossil fuels. Therefore, simple and efficient methods for the extraction and quantification of these compounds become necessary. In this study, a high-performance liquid chromatography-refractive index detection (HPLC-RID) method was developed for the simultaneous quantification of fatty acids and fatty alcohols in these samples. The optimum chromatographic conditions are C18 column eluted with methanol:water:acetic acid (90:9.9:0.1, v/v/v); column temperature, 26°C; flow rate, 1.0mL/min. Calibration curves of all selected analytes showed good linearity (r(2)≥0.9989). The intra-day and inter-day relative standard deviations (RSDs) of the 10 compounds were less than 4.46% and 5.38%, respectively, which indicated that the method had good repeatability and precision. Besides, a method for simultaneous extraction of fatty acids and fatty alcohols from fermentation broth was optimized by orthogonal design. The optimal extraction conditions were as follows: solvent, ethyl acetate; solvent to sample ratio, 0.5:1; rotation speed, 2min at 260rpm; extraction temperature, 10°C. This study provides simple and fast methods to simultaneously extract and quantify fatty acids and fatty alcohols for the first time. It will be useful for the study of microbial production of these products. Copyright © 2013 Elsevier B.V. All rights reserved.

Dual dispersive liquid-liquid microextraction for determination of phenylpropenes in oils by gas chromatography-mass spectrometry.

PubMed

Tsai, Chia-Ju; Li, Jih-Heng; Feng, Chia-Hsien

2015-09-04

A novel, simple and quick sample preparation method was developed and used for pre-concentration and extraction of six phenylpropenes, including anethole, estragole, eugenol, methyl eugenol, safrole and myristicin, from oil samples by dual dispersive liquid-liquid microextraction. Gas chromatography-mass spectrometry was used for determination and separation of compounds. Several experimental parameters affecting extraction efficiency were evaluated and optimized, including forward-extractant type and volume, surfactant type and concentration, water volume, and back-extractant type and volume. For all analytes (10-1000ng/mL), the limits of detection (S/N≧3) ranged from 1.0 to 3.0ng/mL; the limits of quantification (S/N≧10) ranged from 2.5 to 10.0ng/mL; and enrichment factors ranged from 3.2 to 37.1 times. Within-run and between-run relative standard deviations (n=6) were less than 2.61% and less than 4.33%, respectively. Linearity was excellent with determination coefficients (r(2)) above 0.9977. The experiments showed that the proposed method is a simple, effective, and environmentally friendly method of analyzing phenylpropenes in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple and rapid DNA extraction method from whole blood for highly sensitive detection and quantitation of HIV-1 proviral DNA by real-time PCR.

PubMed

McFall, Sally M; Wagner, Robin L; Jangam, Sujit R; Yamada, Douglas H; Hardie, Diana; Kelso, David M

2015-03-01

Early diagnosis and access to treatment for infants with human immunodeficiency virus-1 (HIV-1) is critical to reduce infant mortality. The lack of simple point-of-care tests impedes the timely initiation of antiretroviral therapy. The development of FINA, filtration isolation of nucleic acids, a novel DNA extraction method that can be performed by clinic personnel in less than 2 min has been reported previously. In this report, significant improvements in the DNA extraction and amplification methods are detailed that allow sensitive quantitation of as little as 10 copies of HIV-1 proviral DNA and detection of 3 copies extracted from 100 μl of whole blood. An internal control to detect PCR inhibition was also incorporated. In a preliminary field evaluation of 61 South African infants, the FINA test demonstrated 100% sensitivity and specificity. The proviral copy number of the infant specimens was quantified, and it was established that 100 microliters of whole blood is required for sensitive diagnosis of infants. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

New method for the rapid extraction of natural products: efficient isolation of shikimic acid from star anise.

PubMed

Just, Jeremy; Deans, Bianca J; Olivier, Wesley J; Paull, Brett; Bissember, Alex C; Smith, Jason A

2015-05-15

A new, practical, rapid, and high-yielding process for the pressurized hot water extraction (PHWE) of multigram quantities of shikimic acid from star anise (Illicium verum) using an unmodified household espresso machine has been developed. This operationally simple and inexpensive method enables the efficient and straightforward isolation of shikimic acid and the facile preparation of a range of its synthetic derivatives.

Optimization of microwave-assisted enzymatic extraction of polysaccharides from the fruit of Schisandra chinensis Baill.

PubMed

Cheng, Zhenyu; Song, Haiyan; Yang, Yingjie; Liu, Yan; Liu, Zhigang; Hu, Haobin; Zhang, Yang

2015-05-01

A microwave-assisted enzymatic extraction (MAEE) method had been developed, which was optimized by response surface methodology (RSM) and orthogonal test design, to enhance the extraction of crude polysaccharides (CPS) from the fruit of Schisandra chinensis Baill. The optimum conditions were as follows: microwave irradiation time of 10 min, extraction pH of 4.21, extraction temperature of 47.58°C, extraction time of 3h and enzyme concentration of 1.5% (wt% of S. chinensis powder) for cellulase, papain and pectinase, respectively. Under these conditions, the extraction yield of CPS was 7.38 ± 0.21%, which was well in close agreement with the value predicted by the model. The three methods including heat-refluxing extraction (HRE), ultrasonic-assisted extraction (UAE) and enzyme-assisted extraction (EAE) for extracting CPS by RSM were further compared. Results indicated MAEE method had the highest extraction yields of CPS at lower temperature. It was indicated that the proposed approach in this study was a simple and efficient technique for extraction of CPS in S. chinensis Baill. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Electrochemical extraction of gold from wastes as nanoparticles stabilized by phospholipids.

PubMed

Moriwaki, Hiroshi; Yamada, Kotaro; Usami, Hisanao

2017-02-01

A simple one-step method for the extraction of gold from wastes as nanoparticles stabilized by phospholipids is demonstrated. This is achieved by applying an AC voltage for 5s to the gold-containing wastes, which act as the electrodes in a buffer solution containing a dispersed phospholipid (1,2-dioleoyl-sn-glycero-3-phosphocholine, DOPC). This is an environmentally friendly and rapid method for recovering gold from wastes. The extracted gold nanoparticles have significant potential as a catalyst or biomedical material. Copyright © 2016 Elsevier Ltd. All rights reserved.

Simple Sodium Dodecyl Sulfate-Assisted Sample Preparation Method for LC-MS-based Proteomic Applications

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

Zhou, Jianying; Dann, Geoffrey P.; Shi, Tujin

2012-03-10

Sodium dodecyl sulfate (SDS) is one of the most popular laboratory reagents used for highly efficient biological sample extraction; however, SDS presents a significant challenge to LC-MS-based proteomic analyses due to its severe interference with reversed-phase LC separations and electrospray ionization interfaces. This study reports a simple SDS-assisted proteomic sample preparation method facilitated by a novel peptide-level SDS removal protocol. After SDS-assisted protein extraction and digestion, SDS was effectively (>99.9%) removed from peptides through ion substitution-mediated DS- precipitation with potassium chloride (KCl) followed by {approx}10 min centrifugation. Excellent peptide recovery (>95%) was observed for less than 20 {mu}g of peptides.more » Further experiments demonstrated the compatibility of this protocol with LC-MS/MS analyses. The resulting proteome coverage from this SDS-assisted protocol was comparable to or better than those obtained from other standard proteomic preparation methods in both mammalian tissues and bacterial samples. These results suggest that this SDS-assisted protocol is a practical, simple, and broadly applicable proteomic sample processing method, which can be particularly useful when dealing with samples difficult to solubilize by other methods.« less

RP-HPTLC densitometric determination and validation of vanillin and related phenolic compounds in accelerated solvent extract of Vanilla planifolia*.

PubMed

Sharma, Upendra Kumar; Sharma, Nandini; Gupta, Ajai Prakash; Kumar, Vinod; Sinha, Arun Kumar

2007-12-01

A simple, fast and sensitive RP-HPTLC method is developed for simultaneous quantitative determination of vanillin and related phenolic compounds in ethanolic extracts of Vanilla planifolia pods. In addition to this, the applicability of accelerated solvent extraction (ASE) as an alternative to microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and Soxhlet extraction was also explored for the rapid extraction of phenolic compounds in vanilla pods. Good separation was achieved on aluminium plates precoated with silica gel RP-18 F(254S) in the mobile phase of methanol/water/isopropanol/acetic acid (30:65:2:3, by volume). The method showed good linearity, high precision and good recovery of compounds of interest. ASE showed good extraction efficiency in less time as compared to other techniques for all the phenolic compounds. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

Charge carrier mobility in thin films of organic semiconductors by the gated van der Pauw method

PubMed Central

Rolin, Cedric; Kang, Enpu; Lee, Jeong-Hwan; Borghs, Gustaaf; Heremans, Paul; Genoe, Jan

2017-01-01

Thin film transistors based on high-mobility organic semiconductors are prone to contact problems that complicate the interpretation of their electrical characteristics and the extraction of important material parameters such as the charge carrier mobility. Here we report on the gated van der Pauw method for the simple and accurate determination of the electrical characteristics of thin semiconducting films, independently from contact effects. We test our method on thin films of seven high-mobility organic semiconductors of both polarities: device fabrication is fully compatible with common transistor process flows and device measurements deliver consistent and precise values for the charge carrier mobility and threshold voltage in the high-charge carrier density regime that is representative of transistor operation. The gated van der Pauw method is broadly applicable to thin films of semiconductors and enables a simple and clean parameter extraction independent from contact effects. PMID:28397852

Object extraction method for image synthesis

NASA Astrophysics Data System (ADS)

Inoue, Seiki

1991-11-01

The extraction of component objects from images is fundamentally important for image synthesis. In TV program production, one useful method is the Video-Matte technique for specifying the necessary boundary of an object. This, however, involves some manually intricate and tedious processes. A new method proposed in this paper can reduce the needed level of operator skill and simplify object extraction. The object is automatically extracted by just a simple drawing of a thick boundary line. The basic principle involves a thinning of the thick boundary line binary image using the edge intensity of the original image. This method has many practical advantages, including the simplicity of specifying an object, the high accuracy of thinned-out boundary line, its ease of application to moving images, and the lack of any need for adjustment.

A sensitive method for the determination of Sulfonamides in seawater samples by Solid Phase Extraction and UV-Visible spectrophotometry

NASA Astrophysics Data System (ADS)

Errayess, Sophia Ait; Lahcen, Abdellatif Ait; Idrissi, Laila; Marcoaldi, Caterina; Chiavarini, Salvatore; Amine, Aziz

2017-06-01

The authors have developed a sensitive spectrophotometric method for determination of sulfonamide derivatives such as sulfanilamide (SAA), sulfadiazine (SDZ), sulfacetamide (SCT) sulfamethoxazole (SMX), sulfamerazine (SMR), sulfadimethoxine (SDX), sulfamethiazole (SMT) and Sulfathiazole (STZ). This method is based on the Bratton-Marshall reaction, which involves the diazotization of sulfonamides with sodium nitrite under acidic conditions, followed by coupling with N-(1-naphtyl) ethylenediamine dihydrochloride (NED) to form a pink colored compound. Therefore, the Bratton-Marshall method was modified by optimizing the reaction conditions, which allows us to determine a low concentration range of sulfonamides compared to the reported methods. The limits of detection and quantification obtained were 0.019-0.05 and 0.06-0.16 μg mL- 1, respectively. In comparison with other reported methods using different coupling agents, the proposed method was found to be the most simple and sensitive for sulfonamides determination. In this paper, the modified method was successfully employed for the determination of sulfonamides in drinking water, seawater and pharmaceutical and veterinary formulations. The purpose of this work is to optimize and develop a simple method for extraction and concentration of sulfonamides present as residues in seawater and their quantification with the recommended spectrophotometric method. Solid phase extraction (SPE) of sulfonamides from seawater samples was evaluated using Oasis HLB cartridges (3 mL, 540 mg). The recovery efficiency was investigated in the sulfonamides concentration range comprised between 0.19 and 126 ng mL- 1. The ease of use of this extraction method makes it very useful for routine laboratory work.

Determination of 129I in environmental samples by AMS and NAA using an anion exchange resin disk

NASA Astrophysics Data System (ADS)

Suzuki, Takashi; Banba, Shigeru; Kitamura, Toshikatsu; Kabuto, Shoji; Isogai, Keisuke; Amano, Hikaru

2007-06-01

We have developed a new extraction method for the measurement of 129I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of 129I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

Development and Validation of an Analytical Methodology Based on Liquid Chromatography-Electrospray Tandem Mass Spectrometry for the Simultaneous Determination of Phenolic Compounds in Olive Leaf Extract.

PubMed

Cittan, Mustafa; Çelik, Ali

2018-04-01

A simple method was validated for the analysis of 31 phenolic compounds using liquid chromatography-electrospray tandem mass spectrometry. Proposed method was successfully applied to the determination of phenolic compounds in an olive leaf extract and 24 compounds were analyzed quantitatively. Olive biophenols were extracted from olive leaves by using microwave-assisted extraction with acceptable recovery values between 78.1 and 108.7%. Good linearities were obtained with correlation coefficients over 0.9916 from calibration curves of the phenolic compounds. The limits of quantifications were from 0.14 to 3.2 μg g-1. Intra-day and inter-day precision studies indicated that the proposed method was repeatable. As a result, it was confirmed that the proposed method was highly reliable for determination of the phenolic species in olive leaf extracts.

A simple method for the enrichment of bisphenols using boron nitride.

PubMed

Fischnaller, Martin; Bakry, Rania; Bonn, Günther K

2016-03-01

A simple solid-phase extraction method for the enrichment of 5 bisphenol derivatives using hexagonal boron nitride (BN) was developed. BN was applied to concentrate bisphenol derivatives in spiked water samples and the compounds were analyzed using HPLC coupled to fluorescence detection. The effect of pH and organic solvents on the extraction efficiency was investigated. An enrichment factor up to 100 was achieved without evaporation and reconstitution. The developed method was applied for the determination of bisphenol A migrated from some polycarbonate plastic products. Furthermore, bisphenol derivatives were analyzed in spiked and non-spiked canned food and beverages. None of the analyzed samples exceeded the migration limit set by the European Union of 0.6mg/kg food. The method showed good recovery rates ranging from 80% to 110%. Validation of the method was performed in terms of accuracy and precision. The applied method is robust, fast, efficient and easily adaptable to different analytical problems. Copyright © 2015 Elsevier Ltd. All rights reserved.

GREEN SYNTHESIS OF SILVER AND PALLADIUM NANOPARTICLES AT ROOM TEMPERATURE USING COFFEE AND TEA EXTRACT

EPA Science Inventory

An extremely simple green approach that generates bulk quantities of nanocrystals of noble metals such as silver (Ag) and palladium (Pd) using coffee and tea extract at room temperature is described. The single-pot method uses no surfactant, capping agent, and/or template. The ob...

Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

PubMed

Magiera, Sylwia; Kwietniowska, Ewelina

2016-11-15

In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria.

PubMed

Peng, Li-Qing; Yu, Wen-Yan; Xu, Jing-Jing; Cao, Jun

2018-01-15

A simple, green and effective extraction method, namely, pyridinium ionic liquid- (IL) based liquid-solid extraction (LSE), was first designed to extract the main inorganic and organic iodine compounds (I - , monoiodo-tyrosine (MIT) and diiodo-tyrosine (DIT)). The optimal extraction conditions were as follows: ultrasonic intensity 100W, IL ([EPy]Br) concentration 200mM, extraction time 30min, liquid/solid ratio 10mL/g, and pH value 6.5. The morphologies of Laminaria were studied by scanning electron microscopy and transmission electron microscopy. The recovery values of I - , MIT and DIT from Laminaria were in the range of 88% to 94%, and limits of detection were in the range of 59.40 to 283.6ng/g. The proposed method was applied to the extraction and determination of iodine compounds in three Laminaria. The results showed that IL-based LSE could be a promising method for rapid extraction of bioactive iodine from complex food matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-12-01

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

Methods and systems for detection of radionuclides

DOEpatents

Coates, Jr., John T.; DeVol, Timothy A.

2010-05-25

Disclosed are materials and systems useful in determining the existence of radionuclides in an aqueous sample. The materials provide the dual function of both extraction and scintillation to the systems. The systems can be both portable and simple to use, and as such can beneficially be utilized to determine presence and optionally concentration of radionuclide contamination in an aqueous sample at any desired location and according to a relatively simple process without the necessity of complicated sample handling techniques. The disclosed systems include a one-step process, providing simultaneous extraction and detection capability, and a two-step process, providing a first extraction step that can be carried out in a remote field location, followed by a second detection step that can be carried out in a different location.

Optimization of microwave-assisted extraction for the characterization of olive leaf phenolic compounds by using HPLC-ESI-TOF-MS/IT-MS(2).

PubMed

Taamalli, Amani; Arráez-Román, David; Ibañez, Elena; Zarrouk, Mokhtar; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

2012-01-25

In the present work, a simple and rapid method for the extraction of phenolic compounds from olive leaves, using microwave-assisted extraction (MAE) technique, has been developed. The experimental variables that affect the MAE process, such as the solvent type and composition, microwave temperature, and extraction time, were optimized using a univariate method. The obtained extracts were analyzed by using high-performance liquid chromatography (HPLC) coupled to electrospray time-of-flight mass spectrometry (ESI-TOF-MS) and electrospray ion trap tandem mass spectrometry (ESI-IT-MS(2)) to prove the MAE extraction efficiency. The optimal MAE conditions were methanol:water (80:20, v/v) as extracting solvent, at a temperature equal to 80 °C for 6 min. Under these conditions, several phenolic compounds could be characterized by HPLC-ESI-MS/MS(2). As compared to the conventional method, MAE can be used as an alternative extraction method for the characterization of phenolic compounds from olive leaves due to its efficiency and speed.

Fast and effective low-temperature freezing extraction technique to determine organotin compounds in edible vegetable oil.

PubMed

Liu, Yingxia; Ma, Yaqian; Wan, Yiqun; Guo, Lan; Wan, Xiaofen

2016-06-01

Most organotin compounds that have been widely used in food packaging materials and production process show serious toxicity effects to human health. In this study, a simple and low-cost method based on high-performance liquid chromatography with inductively coupled plasma mass spectrometry for the simultaneous determination of four organotins in edible vegetable oil samples was developed. Four organotins including dibutyltin dichloride, tributyltin chloride, diphenyltin dichloride, and triphenyltin chloride were simultaneously extracted with methanol using the low-temperature precipitation process. After being concentrated, the extracts were purified by matrix solid-phase dispersion using graphitized carbon black. The experimental parameters such as extraction solvent and clean-up material were optimized. To evaluate the accuracy of the new method, the recoveries were investigated. In addition, a liquid chromatography with tandem mass spectrometry method was also proposed for comparison. The procedures of extracting and purifying samples for the analysis were simple and easy to perform batch operations, also showed good efficiency with lower relative standard deviation. The limits of detection of the four organotins were 0.28-0.59 μg/L, and the limits of quantification of the four organotins were 0.93-1.8 μg/L, respectively. The proposed method was successfully applied to the simultaneous analysis of the four organotins in edible vegetable oil. Some analytes were detected at the level of 2.5-28.8 μg/kg. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validation of green-solvent extraction combined with chromatographic chemical fingerprint to evaluate quality of Stevia rebaudiana Bertoni.

PubMed

Teo, Chin Chye; Tan, Swee Ngin; Yong, Jean Wan Hong; Hew, Choy Sin; Ong, Eng Shi

2009-02-01

An approach that combined green-solvent methods of extraction with chromatographic chemical fingerprint and pattern recognition tools such as principal component analysis (PCA) was used to evaluate the quality of medicinal plants. Pressurized hot water extraction (PHWE) and microwave-assisted extraction (MAE) were used and their extraction efficiencies to extract two bioactive compounds, namely stevioside (SV) and rebaudioside A (RA), from Stevia rebaudiana Bertoni (SB) under different cultivation conditions were compared. The proposed methods showed that SV and RA could be extracted from SB using pure water under optimized conditions. The extraction efficiency of the methods was observed to be higher or comparable to heating under reflux with water. The method precision (RSD, n = 6) was found to vary from 1.91 to 2.86% for the two different methods on different days. Compared to PHWE, MAE has higher extraction efficiency with shorter extraction time. MAE was also found to extract more chemical constituents and provide distinctive chemical fingerprints for quality control purposes. Thus, a combination of MAE with chromatographic chemical fingerprints and PCA provided a simple and rapid approach for the comparison and classification of medicinal plants from different growth conditions. Hence, the current work highlighted the importance of extraction method in chemical fingerprinting for the classification of medicinal plants from different cultivation conditions with the aid of pattern recognition tools used.

Validation and Application of a Simple UHPLC–MS-MS Method for the Enantiospecific Determination of Warfarin in Human Urine

PubMed Central

Alshogran, Osama Y.; Ocque, Andrew J.; Leblond, François A.; Pichette, Vincent; Nolin, Thomas D.

2016-01-01

A simple and rapid liquid chromatographic–tandem mass spectrometric method has been developed and validated for the enantiospecific determination of R- and S-warfarin in human urine. Warfarin enantiomers were extracted from urine using methyl tert-butyl ether. Chromatographic separation of warfarin enantiomers and the internal standard d5-warfarin was achieved using a Astec Chirobiotic V column with gradient mobile phase at a flow rate of 400 µL/min over 10 min. Detection was performed on a TSQ Quantum Ultra triple quadrupole mass spectrometer equipped with a heated electrospray ionization source. Analytes were detected in negative ionization mode using selected reaction monitoring. Calibration curves were linear with a correlation coefficient of ≥0.996 for both enantiomers over a concentration range of 5–500 ng/mL. The intra- and interday accuracy and precision for both analytes were within ±9.0%. Excellent extraction efficiency and negligible matrix effects were observed. The applicability of the method was demonstrated by successful measurement of warfarin enantiomers in urine of patients with kidney disease. The method is simple, accurate and reproducible and is currently being used to support warfarin pharmacokinetic studies. PMID:26657732

Simple and rapid analytical method for detection of amino acids in blood using blood spot on filter paper, fast-GC/MS and isotope dilution technique.

PubMed

Kawana, Shuichi; Nakagawa, Katsuhiro; Hasegawa, Yuki; Yamaguchi, Seiji

2010-11-15

A simple and rapid method for quantitative analysis of amino acids, including valine (Val), leucine (Leu), isoleucine (Ile), methionine (Met) and phenylalanine (Phe), in whole blood has been developed using GC/MS. In this method, whole blood was collected using a filter paper technique, and a 1/8 in. blood spot punch was used for sample preparation. Amino acids were extracted from the sample, and the extracts were purified using cation-exchange resins. The isotope dilution method using ²H₈-Val, ²H₃-Leu, ²H₃-Met and ²H₅-Phe as internal standards was applied. Following propyl chloroformate derivatization, the derivatives were analyzed using fast-GC/MS. The extraction recoveries using these techniques ranged from 69.8% to 87.9%, and analysis time for each sample was approximately 26 min. Calibration curves at concentrations from 0.0 to 1666.7 μmol/l for Val, Leu, Ile and Phe and from 0.0 to 333.3 μmol/l for Met showed good linearity with regression coefficients=1. The method detection limits for Val, Leu, Ile, Met and Phe were 24.2, 16.7, 8.7, 1.5 and 12.9 μmol/l, respectively. This method was applied to blood spot samples obtained from patients with phenylketonuria (PKU), maple syrup urine disease (MSUD), hypermethionine and neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), and the analysis results showed that the concentrations of amino acids that characterize these diseases were increased. These results indicate that this method provides a simple and rapid procedure for precise determination of amino acids in whole blood. Copyright © 2010 Elsevier B.V. All rights reserved.

A simple and rapid electrophoretic method to characterize simple phenols, lignans, complex phenols, phenolic acids, and flavonoids in extra-virgin olive oil.

PubMed

Carrasco-Pancorbo, Alegria; Gómez-Caravaca, Ana Maria; Cerretani, Lorenzo; Bendini, Alessandra; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

2006-09-01

We have devised a simple and rapid capillary electrophoretic method which provides the analyst with a useful tool for the characterization of the polyphenolic fraction of extra-virgin olive oil. This method that uses a capillary with 50 microm id and a total length of 47 cm (40 cm to the detector) with a detection window of 100 x 200 microm, and a buffer solution containing 45 mM of sodium tetraborate pH 9.3 offers valuable information about all the families of compounds present in the polar fraction of the olive oil. The detection was carried out by UV absorption at 200, 240, 280, and 330 nm in order to facilitate the identification of the compounds. Concretely, the method permits the identification of simple phenols, lignans, complex phenols (isomeric forms of secoiridoids), phenolic acids, and flavonoids in the SPE-Diol extracts from extra-virgin olive oil in a short time (less than 10 min) and provides a satisfactory resolution. Peak identification was done by comparing both migration time and spectral data obtained from olive oil samples and standards (commercial or isolated (by HPLC-MS) standards), with spiked methanol-water extracts of olive oil with HPLC-collected compounds and commercially available standards at several concentration levels, studying the information of the electropherograms obtained at several wavelengths and also using the information previously reported.

Hormonal profiling: Development of a simple method to extract and quantify phytohormones in complex matrices by UHPLC-MS/MS.

PubMed

Delatorre, Carolina; Rodríguez, Ana; Rodríguez, Lucía; Majada, Juan P; Ordás, Ricardo J; Feito, Isabel

2017-01-01

Plant growth regulators (PGRs) are very different chemical compounds that play essential roles in plant development and the regulation of physiological processes. They exert their functions by a mechanism called cross-talk (involving either synergistic or antagonistic actions) thus; it is for great interest to study as many PGRs as possible to obtain accurate information about plant status. Much effort has been applied to develop methods capable of analyze large numbers of these compounds but frequently excluding some chemical families or important PGRs within each family. In addition, most of the methods are specially designed for matrices easy to work with. Therefore, we wanted to develop a method which achieved the requirements lacking in the literature and also being fast and reliable. Here we present a simple, fast and robust method for the extraction and quantification of 20 different PGRs using UHPLC-MS/MS optimized in complex matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

Microburger Biochemistry: Extraction and Spectral Characterization of Myoglyobin from Hamburger

NASA Astrophysics Data System (ADS)

Bylkas, Sheri A.; Andersson, Laura A.

1997-04-01

This experiment provides a demonstration of useful biochemical methods at a Basic or Advanced Level, depending upon the available spectrophotometric equipment. The protocol combines protein extraction, ox-i-dation and reduction, and simple spectroscopic analysis, as well as gel filtration chromatography and generation/analysis of spectral scans. Mammalian myoglobin (Mb) is a monomeric O2-binding protein that functions in muscle to store oxygen. The single iron protoporphyrin IX (heme) group is bound to protein by the amino acid Histidine93. The common, stable forms, Met-Mb and Oxy-Mb are studied because in a non-living system, red Oxy-Mb is converted to brown Met-Mb as bound O2 molecule is released. Mb is easily extracted from steak, to illustrate and address why fresh meat is red and aged meat is brown; the protein has unique spectral properties that are diagnostic for characterization of sample identity. After application of heme redox chemical methods, the MetMb or OxyMb samples can be studied spectroscopically. The color change between Oxy-Mb and Met-Mb is dramatic (illustrating bright red fresh meat vs. brown older meat), and method(s) used in this laboratory are simple, inexpensive, and non-harmful to the student.

Evaluation of a QuECHERS-like extraction approach for the determination of PBDEs in mussels by immuno-assay-based screening methods

USDA-ARS?s Scientific Manuscript database

A sample preparation method was evaluated for the determination of polybrominated diphenyl ethers (PBDEs) in mussel samples, by using colorimetric and electrochemical immunoassay-based screening methods. A simple sample preparation in conjunction with a rapid screening method possesses the desired c...

Microwave-assisted extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb.

PubMed

Zhang, Fan; Yang, Yi; Su, Ping; Guo, Zhenku

2009-01-01

Euonymus alatus (Thunb.) has been used as one of traditional Chinese medicines for several thousand years. Conventional methods for the extraction of rutin and quercetin from E. alatus, including solvent extraction, Soxhlet extraction and heat reflux extraction are characterised by long extraction times and consumption of large amounts of solvents. To develop a simple and rapid method for the extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb using microwave-assisted extraction (MAE) technique. MAE experiments were performed with a multimode microwave extraction system. The experimental variables that affect the MAE process, such as the concentration of ethanol solution, extractant volume, microwave power and extraction time were optimised. Yields were determined by HPLC. The results were compared with that obtained by classical Soxhlet and ultrasonic-assisted extraction (UAE). From the optimised conditions for MAE of rutin and quercetin it can be concluded that the solvent is 50% ethanol (v/v) solution, the extractant volume is 40 mL, microwave power is 170 W and irradiation time is 6 min. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction is a rapid method with a higher yield and lower solvent consumption. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

Determination of free sulfites (SO3-2) in dried fruits processed with sulfur dioxide by ion chromatography through anion exchange column and conductivity detection.

PubMed

Liao, Benjamin S; Sram, Jacqueline C; Files, Darin J

2013-01-01

A simple and effective anion ion chromatography (IC) method with anion exchange column and conductivity detector has been developed to determine free sulfites (SO3-2) in dried fruits processed with sulfur dioxide. No oxidation agent, such as hydrogen peroxide, is used to convert sulfites to sulfates for IC analysis. In addition, no stabilizing agent, such as formaldehyde, fructose or EDTA, is required during the sample extraction. This method uses aqueous 0.2 N NaOH as the solvent for standard preparation and sample extraction. The sulfites, either prepared from standard sodium sulfite powder or extracted from food samples, are presumed to be unbound SO3-2 in aqueous 0.2 N NaOH (pH > 13), because the bound sulfites in the sample matrix are released at pH > 10. In this study, sulfites in the standard solutions were stable at room temperature (i.e., 15-25 degrees C) for up to 12 days. The lowest standard of the linear calibration curve is set at 1.59 microg/mL SO3-2 (equivalent to 6.36 microg/g sample with no dilution) for analysis of processed dried fruits that would contain high levels (>1000 microg/g) of sulfites. As a consequence, this method typically requires significant dilution of the sample extract. Samples are prepared with a simple procedure of sample compositing, extraction with aqueous 0.2 N NaOH, centrifugation, dilution as needed, and filtration prior to IC. The sulfites in these sample extracts are stable at room temperature for up to 20 h. Using anion IC, the sulfites are eluted under isocratic conditions with 10 mM aqueous sodium carbonate solution as the mobile phase passing through an anion exchange column. The sulfites are easily separated, with an analysis run time of 18 min, regardless of the dried fruit matrix. Recoveries from samples spiked with sodium sulfites were demonstrated to be between 81 and 105% for five different fruit matrixes (apricot, golden grape, white peach, fig, and mango). Overall, this method is simple to perform and effective for the determination of high levels of sulfites in dried fruits.

Classification of epileptic EEG signals based on simple random sampling and sequential feature selection.

PubMed

Ghayab, Hadi Ratham Al; Li, Yan; Abdulla, Shahab; Diykh, Mohammed; Wan, Xiangkui

2016-06-01

Electroencephalogram (EEG) signals are used broadly in the medical fields. The main applications of EEG signals are the diagnosis and treatment of diseases such as epilepsy, Alzheimer, sleep problems and so on. This paper presents a new method which extracts and selects features from multi-channel EEG signals. This research focuses on three main points. Firstly, simple random sampling (SRS) technique is used to extract features from the time domain of EEG signals. Secondly, the sequential feature selection (SFS) algorithm is applied to select the key features and to reduce the dimensionality of the data. Finally, the selected features are forwarded to a least square support vector machine (LS_SVM) classifier to classify the EEG signals. The LS_SVM classifier classified the features which are extracted and selected from the SRS and the SFS. The experimental results show that the method achieves 99.90, 99.80 and 100 % for classification accuracy, sensitivity and specificity, respectively.

Extraction of Curcumin Pigment from Indonesian Local Turmeric with Its Infrared Spectra and Thermal Decomposition Properties

NASA Astrophysics Data System (ADS)

Nandiyanto, A. B. D.; Wiryani, A. S.; Rusli, A.; Purnamasari, A.; Abdullah, A. G.; Ana; Widiaty, I.; Hurriyati, R.

2017-03-01

Curcumin is one of the pigments which is used as a spice in Asian cuisine, traditional cosmetic, and medicine. Therefore, process for getting curcumin has been widely studied. Here, the purpose of this study was to demonstrate the simple method for extracting curcumin from Indonesian local turmeric and investigate the infrared spectra and thermal decomposition properties. In the experimental procedure, the washed turmeric was dissolved into an ethanol solution, and then put into a rotary evaporator to enrich curcumin concentration. The result showed that the present method is effective to isolate curcumin compound from Indonesian local turmeric. Since the process is very simple, this method can be used for home industrial application. Further, understanding the thermal decomposition properties of curcumin give information, specifically relating to the selection of treatment when curcumin must face the thermal-related process.

Simultaneous dispersive liquid-liquid microextraction derivatisation and gas chromatography mass spectrometry analysis of subcritical water extracts of sweet and sour cherry stems.

PubMed

Švarc-Gajić, Jaroslava; Clavijo, Sabrina; Suárez, Ruth; Cvetanović, Aleksandra; Cerdà, Víctor

2018-03-01

Cherry stems have been used in traditional medicine mostly for the treatment of urinary tract infections. Extraction with subcritical water, according to its selectivity, efficiency and other aspects, differs substantially from conventional extraction techniques. The complexity of plant subcritical water extracts is due to the ability of subcritical water to extract different chemical classes of different physico-chemical properties and polarities in a single run. In this paper, dispersive liquid-liquid microextraction (DLLME) with simultaneous derivatisation was optimised for the analysis of complex subcritical water extracts of cherry stems to allow simple and rapid preparation prior to gas chromatography-mass spectrometry (GC-MS). After defining optimal extracting and dispersive solvents, the optimised method was used for the identification of compounds belonging to different chemical classes in a single analytical run. The developed sample preparation protocol enabled simultaneous extraction and derivatisation, as well as convenient coupling with GC-MS analysis, reducing the analysis time and number of steps. The applied analytical protocol allowed simple and rapid chemical screening of subcritical water extracts and was used for the comparison of subcritical water extracts of sweet and sour cherry stems. Graphical abstract DLLME GC MS analysis of cherry stem extracts obtained by subcritical water.

A rapid and simple method for estimating sulfate reduction activity and quantifying inorganic sulfides

USGS Publications Warehouse

Ulrich, G.A.; Krumholz, L.R.; Suflita, J.M.

1997-01-01

A simplified passive extraction procedure for quantifying reduced inorganic sulfur compounds from sediments and water is presented. This method may also be used for the estimation of sulfate reduction rates. Efficient extraction of FeS, FeS(inf2), and S(sup2-) was obtained with this procedure; however, the efficiency for S(sup0) depended on the form that was tested. Passive extraction can be used with samples containing up to 20 mg of reduced sulfur. We demonstrated the utility of this technique in a determination of both sulfate reduction rates and reduced inorganic sulfur pools in marine and freshwater sediments. A side-by-side comparison of the passive extraction method with the established single-step distillation technique yielded comparable results with a fraction of the effort.

Method for Face-Emotion Retrieval Using A Cartoon Emotional Expression Approach

NASA Astrophysics Data System (ADS)

Kostov, Vlaho; Yanagisawa, Hideyoshi; Johansson, Martin; Fukuda, Shuichi

A simple method for extracting emotion from a human face, as a form of non-verbal communication, was developed to cope with and optimize mobile communication in a globalized and diversified society. A cartoon face based model was developed and used to evaluate emotional content of real faces. After a pilot survey, basic rules were defined and student subjects were asked to express emotion using the cartoon face. Their face samples were then analyzed using principal component analysis and the Mahalanobis distance method. Feature parameters considered as having relations with emotions were extracted and new cartoon faces (based on these parameters) were generated. The subjects evaluated emotion of these cartoon faces again and we confirmed these parameters were suitable. To confirm how these parameters could be applied to real faces, we asked subjects to express the same emotions which were then captured electronically. Simple image processing techniques were also developed to extract these features from real faces and we then compared them with the cartoon face parameters. It is demonstrated via the cartoon face that we are able to express the emotions from very small amounts of information. As a result, real and cartoon faces correspond to each other. It is also shown that emotion could be extracted from still and dynamic real face images using these cartoon-based features.

Cloud-point extraction and reversed-phase high-performance liquid chromatography for the determination of synthetic phenolic antioxidants in edible oils.

PubMed

Chen, Miao; Xia, Qinghai; Liu, Mousheng; Yang, Yaling

2011-01-01

A cloud-point extraction (CPE) method using Triton X-114 (TX-114) nonionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) from edible oils. The optimum conditions of CPE were 2.5% (v/v) TX-114, 0.5% (w/v) NaCl and 40 min equilibration time at 50 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography with ultraviolet detection at 280 nm, using a gradient mobile phase consisting of methanol and 1.5% (v/v) acetic acid. Under the studied conditions, 4 synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. The limits of detection (LOD) were 1.9 ng mL(-1) for PG, 11 ng mL(-1) for TBHQ, 2.3 ng mL(-1) for BHA, and 5.9 ng mL(-1) for BHT. Recoveries of the SPAs spiked into edible oil were in the range 81% to 88%. The CPE method was shown to be potentially useful for the preconcentration of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes much less solvent than traditional methods, and is environment-friendly. Practical Application: The method established in this article uses less organic solvent to extract SPAs from edible oils; it is simple, highly sensitive and results in no pollution to the environment.

An effective vacuum assisted extraction method for the optimization of labdane diterpenoids from Andrographis paniculata by response surface methodology.

PubMed

Wang, Ya-Qi; Wu, Zhen-Feng; Ke, Gang; Yang, Ming

2014-12-31

An effective vacuum assisted extraction (VAE) technique was proposed for the first time and applied to extract bioactive components from Andrographis paniculata. The process was carefully optimized by response surface methodology (RSM). Under the optimized experimental conditions, the best results were obtained using a boiling temperature of 65 °C, 50% ethanol concentration, 16 min of extraction time, one extraction cycles and a 12:1 liquid-solid ratio. Compared with conventional ultrasonic assisted extraction and heat reflux extraction, the VAE technique gave shorter extraction times and remarkable higher extraction efficiency, which indicated that a certain degree of vacuum gave the solvent a better penetration of the solvent into the pores and between the matrix particles, and enhanced the process of mass transfer. The present results demonstrated that VAE is an efficient, simple and fast method for extracting bioactive components from A. paniculata, which shows great potential for becoming an alternative technique for industrial scale-up applications.

Rapid and Efficient Isolation of High-Quality Small RNAs from Recalcitrant Plant Species Rich in Polyphenols and Polysaccharides

PubMed Central

Pu, Jinji; Guo, Jianrong; Fan, Zaifeng

2014-01-01

Small RNAs, including microRNAs (miRNAs) and small interfering RNAs (siRNAs), are important regulators of plant development and gene expression. The acquisition of high-quality small RNAs is the first step in the study of its expression and function analysis, yet the extraction method of small RNAs in recalcitrant plant tissues with various secondary metabolites is not well established, especially for tropical and subtropical plant species rich in polysaccharides and polyphenols. Here, we developed a simple and efficient method for high quality small RNAs extraction from recalcitrant plant species. Prior to RNA isolation, a precursory step with a CTAB-PVPP buffer system could efficiently remove compounds and secondary metabolites interfering with RNAs from homogenized lysates. Then, total RNAs were extracted by Trizol reagents followed by a differential precipitation of high-molecular-weight (HMW) RNAs using polyethylene glycol (PEG) 8000. Finally, small RNAs could be easily recovered from supernatant by ethanol precipitation without extra elimination steps. The isolated small RNAs from papaya showed high quality through a clear background on gel and a distinct northern blotting signal with miR159a probe, compared with other published protocols. Additionally, the small RNAs extracted from papaya were successfully used for validation of both predicted miRNAs and the putative conserved tasiARFs. Furthermore, the extraction method described here was also tested with several other subtropical and tropical plant tissues. The purity of the isolated small RNAs was sufficient for such applications as end-point stem-loop RT-PCR and northern blotting analysis, respectively. The simple and feasible extraction method reported here is expected to have excellent potential for isolation of small RNAs from recalcitrant plant tissues rich in polyphenols and polysaccharides. PMID:24787387

A simple purification and activity assay of the coagulant protein from Moringa oleifera seed.

PubMed

Ghebremichael, Kebreab A; Gunaratna, K R; Henriksson, Hongbin; Brumer, Harry; Dalhammar, Gunnel

2005-06-01

Use of extracts from Moringa oleifera (MO) is of great interest for low-cost water treatment. This paper discusses water and salt extraction of a coagulant protein from the seed, purification using ion exchange, its chemical characteristics, coagulation and antimicrobial properties. The coagulant from both extracts is a cationic protein with pI greater than 9.6 and molecular mass less than 6.5 kDa. Mass spectrometric analysis of the purified water extract indicated that it contained at least four homologous proteins, based on MS/MS peptide sequence data. The protein is thermoresistant and remained active after 5h heat treatment at 95 degrees C. The coagulant protein showed both flocculating and antibacterial effects of 1.1--4 log reduction. With samples of high turbidity, the MO extract showed similar coagulation activity as alum. Cecropin A and MO extract were found to have similar flocculation effects for clay and microorganisms. Simple methods for both the purification and assay of MO coagulating proteins are presented, which are necessary for large-scale water treatment applications.

An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

PubMed

Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

2009-12-01

An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSD<5.2%. The convention heating reflux extraction was also conducted in order to validate the reliability of this new FMAE method. The yield of total steroidal saponins was 90.3% in a one-step FMAE, while the yield of 65.0% was achieved during heating reflux extraction, and the extraction time was reduced from 3 h to 5 min by using less solvent. The method was successfully applied to analyze the steroidal saponins of Tribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography-tandem mass spectrometry.

PubMed

Dasenaki, Marilena E; Thomaidis, Nikolaos S

2015-06-23

A simple and sensitive multi-residue method for the determination of 115 veterinary drugs and pharmaceuticals, belonging in more than 20 different classes, in butter, milk powder, egg and fish tissue has been developed. The method involves a simple generic solid-liquid extraction step (solvent extraction, SE) with 0.1% formic acid in aqueous solution of EDTA 0.1% (w/v)-acetonitrile (ACN)-methanol (MeOH) (1:1:1, v/v) with additional ultrasonic-assisted extraction. Precipitation of lipids and proteins was promoted by subjecting the extracts at very low temperature (-23°C) for 12h. Further cleanup with hexane ensures fat removal from the matrix. Analysis was performed by liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). Two separate runs were performed for positive and negative ionization in multiple reaction monitoring mode (MRM). Particular attention was devoted to extraction optimization: different sample-to-extracting volume ratios, different concentrations of formic acid in the extraction solvent and different ultrasonic extraction temperatures were tested in butter, egg and milk powder samples. The method was also applied in fish tissue samples. It was validated, on the basis of international guidelines, for all four matrices. Quantitative analysis was performed by means of standard addition calibration. For over 80% of the analytes, the recoveries were between 50% and 120% in all matrices studied, with RSD values in the range of 1-18%. Limits of detection (LODs) and quantification (LOQs) ranged from 0.008 μg kg(-1) (oxfendazole in butter) to 3.15 μg kg(-1) (hydrochlorthiazide in egg). The evaluated method provides reliable screening, quantification, and identification of 115 veterinary drug and pharmaceutical residues in foods of animal origin and has been successfully applied in real samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous Chloramphenicol and Florfenicol Determination by A Validated DLLME-HPLC-UV Method in Pasteurized Milk.

PubMed

Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad

2016-01-01

The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1-79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected.

Simultaneous Chloramphenicol and Florfenicol Determination by A Validated DLLME-HPLC-UV Method in Pasteurized Milk

PubMed Central

Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad

2016-01-01

The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1–79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected. PMID:27980571

A new blood vessel extraction technique using edge enhancement and object classification.

PubMed

Badsha, Shahriar; Reza, Ahmed Wasif; Tan, Kim Geok; Dimyati, Kaharudin

2013-12-01

Diabetic retinopathy (DR) is increasing progressively pushing the demand of automatic extraction and classification of severity of diseases. Blood vessel extraction from the fundus image is a vital and challenging task. Therefore, this paper presents a new, computationally simple, and automatic method to extract the retinal blood vessel. The proposed method comprises several basic image processing techniques, namely edge enhancement by standard template, noise removal, thresholding, morphological operation, and object classification. The proposed method has been tested on a set of retinal images. The retinal images were collected from the DRIVE database and we have employed robust performance analysis to evaluate the accuracy. The results obtained from this study reveal that the proposed method offers an average accuracy of about 97 %, sensitivity of 99 %, specificity of 86 %, and predictive value of 98 %, which is superior to various well-known techniques.

A direct method of extracting surface recombination velocity from an electron beam induced current line scan

NASA Astrophysics Data System (ADS)

Ong, Vincent K. S.

1998-04-01

The extraction of diffusion length and surface recombination velocity in a semiconductor with the use of an electron beam induced current line scan has traditionally been done by fitting the line scan into complicated theoretical equations. It was recently shown that a much simpler equation is sufficient for the extraction of diffusion length. The linearization coefficient is the only variable that is needed to be adjusted in the curve fitting process. However, complicated equations are still necessary for the extraction of surface recombination velocity. It is shown in this article that it is indeed possible to extract surface recombination velocity with a simple equation, using only one variable, the linearization coefficient. An intuitive feel for the reason behind the method was discussed. The accuracy of the method was verified with the use of three-dimensional computer simulation, and was found to be even slightly better than that of the best existing method.

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

PubMed Central

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

2016-01-01

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

A simple rapid process for semi-automated brain extraction from magnetic resonance images of the whole mouse head.

PubMed

Delora, Adam; Gonzales, Aaron; Medina, Christopher S; Mitchell, Adam; Mohed, Abdul Faheem; Jacobs, Russell E; Bearer, Elaine L

2016-01-15

Magnetic resonance imaging (MRI) is a well-developed technique in neuroscience. Limitations in applying MRI to rodent models of neuropsychiatric disorders include the large number of animals required to achieve statistical significance, and the paucity of automation tools for the critical early step in processing, brain extraction, which prepares brain images for alignment and voxel-wise statistics. This novel timesaving automation of template-based brain extraction ("skull-stripping") is capable of quickly and reliably extracting the brain from large numbers of whole head images in a single step. The method is simple to install and requires minimal user interaction. This method is equally applicable to different types of MR images. Results were evaluated with Dice and Jacquard similarity indices and compared in 3D surface projections with other stripping approaches. Statistical comparisons demonstrate that individual variation of brain volumes are preserved. A downloadable software package not otherwise available for extraction of brains from whole head images is included here. This software tool increases speed, can be used with an atlas or a template from within the dataset, and produces masks that need little further refinement. Our new automation can be applied to any MR dataset, since the starting point is a template mask generated specifically for that dataset. The method reliably and rapidly extracts brain images from whole head images, rendering them useable for subsequent analytical processing. This software tool will accelerate the exploitation of mouse models for the investigation of human brain disorders by MRI. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple and rapid DNA extraction method for Chlamydia trachomatis detection from urogenital swabs.

PubMed

Butzler, Matthew A; Reed, Jennifer L; McFall, Sally M

2017-11-01

A highly sensitive and specific Chlamydia trachomatis (CT) diagnostic test was developed by combining filtration isolation of nucleic acid (FINA) extraction with quantitative polymerase chain reaction including an internal control to identify test inhibition. A pilot study of 40 clinical specimens yielded 100% sensitivity and specificity. Copyright © 2017 Elsevier Inc. All rights reserved.

Application of Ionic Liquids in the Microwave-Assisted Extraction of Proanthocyanidins from Larix gmelini Bark

PubMed Central

Yang, Lei; Sun, Xiaowei; Yang, Fengjian; Zhao, Chunjian; Zhang, Lin; Zu, Yuangang

2012-01-01

Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation. PMID:22606036

Extracting Drug-Drug Interactions with Word and Character-Level Recurrent Neural Networks

PubMed Central

Kavuluru, Ramakanth; Rios, Anthony; Tran, Tung

2017-01-01

Drug-drug interactions (DDIs) are known to be responsible for nearly a third of all adverse drug reactions. Hence several current efforts focus on extracting signal from EMRs to prioritize DDIs that need further exploration. To this end, being able to extract explicit mentions of DDIs in free text narratives is an important task. In this paper, we explore recurrent neural network (RNN) architectures to detect and classify DDIs from unstructured text using the DDIExtraction dataset from the SemEval 2013 (task 9) shared task. Our methods are in line with those used in other recent deep learning efforts for relation extraction including DDI extraction. However, to our knowledge, we are the first to investigate the potential of character-level RNNs (Char-RNNs) for DDI extraction (and relation extraction in general). Furthermore, we explore a simple but effective model bootstrapping method to (a). build model averaging ensembles, (b). derive confidence intervals around mean micro-F scores (MMF), and (c). assess the average behavior of our methods. Without any rule based filtering of negative examples, a popular heuristic used by most earlier efforts, we achieve an MMF of 69.13. By adding simple replicable heuristics to filter negative instances we are able to achieve an MMF of 70.38. Furthermore, our best ensembles produce micro F-scores of 70.81 (without filtering) and 72.13 (with filtering), which are superior to metrics reported in published results. Although Char-RNNs turnout to be inferior to regular word based RNN models in overall comparisons, we find that ensembling models from both architectures results in nontrivial gains over simply using either alone, indicating that they complement each other. PMID:29034375

Validated reversed phase LC method for quantitative analysis of polymethoxyflavones in citrus peel extracts.

PubMed

Wang, Zhenyu; Li, Shiming; Ferguson, Stephen; Goodnow, Robert; Ho, Chi-Tang

2008-01-01

Polymethoxyflavones (PMFs), which exist exclusively in the citrus genus, have biological activities including anti-inflammatory, anticarcinogenic, and antiatherogenic properties. A validated RPLC method was developed for quantitative analysis of six major PMFs, namely nobiletin, tangeretin, sinensetin, 5,6,7,4'-tetramethoxyflavone, 3,5,6,7,3',4'-hexamethoxyflavone, and 3,5,6,7,8,3',4'-heptamethoxyflavone. The polar embedded LC stationary phase was able to fully resolve the six analogues. The developed method was fully validated in terms of linearity, accuracy, precision, sensitivity, and system suitability. The LOD of the method was calculated as 0.15 microg/mL and the recovery rate was between 97.0 and 105.1%. This analytical method was successfully applied to quantify the individual PMFs in four commercially available citrus peel extracts (CPEs). Each extract shows significant difference in the PMF composition and concentration. This method may provide a simple, rapid, and reliable tool to help reveal the correlation between the bioactivity of the PMF extracts and the individual PMF content.

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 simple assay for the simultaneous determination of human plasma albendazole and albendazole sulfoxide levels by high performance liquid chromatography in tandem mass spectrometry with solid-phase extraction.

PubMed

Wojnicz, Aneta; Cabaleiro-Ocampo, Teresa; Román-Martínez, Manuel; Ochoa-Mazarro, Dolores; Abad-Santos, Francisco; Ruiz-Nuño, Ana

2013-11-15

A simple, reproducible and fast (4 min chromatogram) method of liquid chromatography in tandem with mass spectrometry (LC/MS-MS) was developed to determine simultaneously the plasma levels of albendazole (ABZ) and its metabolite albendazole sulfoxide (ABZOX) for pharmacokinetic and clinical analysis. Each plasma sample was extracted by solid phase extraction (SPE) using phenacetin as internal standard (IS). The extracted sample was eluted with a Zorbax XDB-CN column using an isocratic method. The mobile phase consisting of water with 1% acetic acid (40%, A) and MeOH (60%, B), was used at a flow rate of 1 mL/min. ABZ and ABZOX were detected and identified by mass spectrometry with electrospray ionization (ESI) in the positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 5-1000 ng/mL for ABZ and 10-1500 ng/mL (full validation) or 10-5000 ng/mL (partial validation) for ABZOX, with 5 and 10 ng/mL lower limit of quantification (LLOQ) for ABZ and ABZOX, respectively. The tests of accuracy and precision, matrix effect, extraction recovery and stability of the samples for both ABZ and ABZOX did not deviate more than 20% for the LLOQ and no more than 15% for other quality controls (QCs), according to regulatory agencies. © 2013.

Extraction of intracellular protein from Glaciozyma antarctica for proteomics analysis

NASA Astrophysics Data System (ADS)

Faizura, S. Nor; Farahayu, K.; Faizal, A. B. Mohd; Asmahani, A. A. S.; Amir, R.; Nazalan, N.; Diba, A. B. Farah; Muhammad, M. Nor; Munir, A. M. Abdul

2013-11-01

Two preparation methods of crude extracts of psychrophilic yeast Glaciozyma antarctica were compared in order to obtain a good recovery of intracellular proteins. Extraction with mechanical procedures using sonication was found to be more effective for obtaining good yield compare to alkaline treatment method. The procedure is simple, rapid, and produce better yield. A total of 52 proteins were identified by combining both extraction methods. Most of the proteins identified in this study involves in the metabolic process including glycolysis pathway, pentose phosphate pathway, pyruyate decarboxylation and also urea cyle. Several chaperons were identified including probable cpr1-cyclophilin (peptidylprolyl isomerase), macrolide-binding protein fkbp12 and heat shock proteins which were postulate to accelerate proper protein folding. Characteristic of the fundamental cellular processes inferred from the expressed-proteome highlight the evolutionary and functional complexity existing in this domain of life.

One-step liquid-liquid extraction of cocaine from urine samples for gas chromatographic analysis.

PubMed

Farina, Marcelo; Yonamine, Maurício; Silva, Ovandir A

2002-07-17

An improved technique for cocaine extraction from urine samples for gas chromatographic (GC) analysis is described. Employing a simple liquid-liquid extraction (LLE) of cocaine with a mixture of ethyl ether:isopropanol (9:1) the method presents a mean recovery of 74.49%. Limit of detection (LOD) and limit of quantification (LOQ) were 5 and 20 ng/ml, respectively. The method is highly precise (coefficient of variation (CV) <8%) and linear from 20 to 2000 ng/ml. It can he applied to detect the presence of cocaine in urine as a marker of its recent use in drug abuse treatment protocols.

A Novel Selective Deep Eutectic Solvent Extraction Method for Versatile Determination of Copper in Sediment Samples by ICP-OES.

PubMed

Bağda, Esra; Altundağ, Huseyin; Tüzen, Mustafa; Soylak, Mustafa

2017-08-01

In the present study, a simple, mono step deep eutectic solvent (DES) extraction was developed for selective extraction of copper from sediment samples. The optimization of all experimental parameters, e.g. DES type, sample/DES ratio, contact time and temperature were performed with using BCR-280 R (lake sediment certified reference material). The limit of detection (LOD) and the limit of quantification (LOQ) were found as 1.2 and 3.97 µg L -1 , respectively. The RSD of the procedure was 7.5%. The proposed extraction method was applied to river and lake sediments sampled from Serpincik, Çeltek, Kızılırmak (Fadl and Tecer region of the river), Sivas-Turkey.

Quantitative determination of 5-hydroxy-N-methylpyrrolidone in urine for biological monitoring of N-methylpyrrolidone exposure.

PubMed

Ligocka, D; Lison, D; Haufroid, V

2002-10-05

The aim of this work was to validate a sensitive method for quantitative analysis of 5-hydroxy-N-methylpyrrolidone (5-HNMP) in urine. This compound has been recommended as a marker for biological monitoring of N-methylpyrrolidone (NMP) exposure. Different solvents and alternative methods of extraction including liquid-liquid extraction (LLE) on Chem Elut and solid-phase extraction (SPE) on Oasis HLB columns were tested. The most efficient extraction of 5-HNMP in urine was LLE with Chem Elut columns and dichloromethane as a solvent (consistently 22% of recovery). The urinary extracts were derivatized by bis(trimethylsilyl)trifluoroacetamide and analysed by gas chromatography-mass spectrometry (GC-MS) with tetradeutered 5-HNMP as an internal standard. The detection limit of this method is 0.017 mg/l urine with an intraassay precision of 1.6-2.6%. The proposed method of extraction is simple and reproducible. Four different m/z signal ratios of TMS-5-HNMP and tetralabelled TMS-5-HNMP have been validated and could be indifferently used in case of unexpected impurities from urine matrix. Copyright 2002 Elsevier Science B.V.

Simultaneous determination of flubendiamide its metabolite desiodo flubendiamide residues in cabbage, tomato and pigeon pea by HPLC.

PubMed

Paramasivam, M; Banerjee, Hemanta

2011-10-01

A sensitive and simple method for simultaneous analysis of flubendiamide and its metabolite desiodo flubendiamide in cabbage, tomato and pigeon pea has been developed. The residues were extracted with QuEChERS method followed by dispersive solid-phase extraction with primary secondary amine sorbent to remove co extractives, prior to analysis by HPLC coupled with UV-Vis detector. The recoveries of flubendiamide and desiodo flubendiamide were ranged from 85.1 to 98.5% and 85.9 to 97.1% respectively with relative standard deviations (RSD) less than 5% and sensitivity of 0.01 μg g(-1). The method offers a less expensive and safer alternative to the existing residue analysis methods for vegetables. © Springer Science+Business Media, LLC 2011

Evaluation of an alternative extraction procedure for enterotoxin determination in dairy products.

PubMed

Meyrand, A; Atrache, V; Bavai, C; Montet, M P; Vernozy-Rozand, C

1999-06-01

A concentration protocol based on trichloroacetic acid precipitation was evaluated and compared with the reference method using dialysis concentration. Different quantities of purified staphylococcal enterotoxins were added to pasteurized Camembert-type cheeses. Detection of enterotoxins in these cheeses was performed using an automated detection system. Raw goat milk Camembert-type cheeses involved in a staphylococcal food poisoning were also tested. Both enterotoxin extraction methods allowed detection of the lowest enterotoxin concentration level used in this study (0.5 ng g-1). Compared with the dialysis concentration method, TCA precipitation of staphylococcal enterotoxins was 'user-friendly' and less time-consuming. These results suggest that TCA precipitation is a rapid (1 h), simple and reliable method of extracting enterotoxin from food which gives excellent recovery from dairy products.

Validation and Application of a Simple UHPLC-MS-MS Method for the Enantiospecific Determination of Warfarin in Human Urine.

PubMed

Alshogran, Osama Y; Ocque, Andrew J; Leblond, François A; Pichette, Vincent; Nolin, Thomas D

2016-04-01

A simple and rapid liquid chromatographic-tandem mass spectrometric method has been developed and validated for the enantiospecific determination of R- and S-warfarin in human urine. Warfarin enantiomers were extracted from urine using methyl tert-butyl ether. Chromatographic separation of warfarin enantiomers and the internal standard d5-warfarin was achieved using a Astec Chirobiotic V column with gradient mobile phase at a flow rate of 400 µL/min over 10 min. Detection was performed on a TSQ Quantum Ultra triple quadrupole mass spectrometer equipped with a heated electrospray ionization source. Analytes were detected in negative ionization mode using selected reaction monitoring. Calibration curves were linear with a correlation coefficient of ≥0.996 for both enantiomers over a concentration range of 5-500 ng/mL. The intra- and interday accuracy and precision for both analytes were within ±9.0%. Excellent extraction efficiency and negligible matrix effects were observed. The applicability of the method was demonstrated by successful measurement of warfarin enantiomers in urine of patients with kidney disease. The method is simple, accurate and reproducible and is currently being used to support warfarin pharmacokinetic studies. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS).

PubMed

Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

2015-11-01

A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.

"One-pot" ethyl chloroformate derivatization and liquid-liquid extraction of reduced glutathione in erythrocyte and its quantitative GC-MS analysis.

PubMed

Manca, Alessandra; Alladio, Eugenio; Massarenti, Paola; Puccinelli, M Paola; De Francesco, Antonella; Del Grosso, Erika; Mengozzi, Giulio; Pazzi, Marco; Vincenti, Marco

2017-12-01

A simple "one-pot" derivatization and liquid-liquid extraction (LLE) procedure was developed for GC-MS analysis of reduced glutathione (GSH) analysis in erythrocytes. The metabolite was extracted by 5% (w/v) TCA, the supernatant treated with ECF and ethanol-pyridine media, the derivative separated and detected by gas chromatography-mass spectrometry using a short non-polar capillary GC column at a high column-head pressure. Total analysis time was 11min. The process was optimized by a Design of Experiment. The method was validated showing a good linearity over the 25.4-813.4μM concentration range, providing satisfactory results in terms of intra-day and inter-day precision as well as an optimal accuracy. The new method was evaluated in a pilot study involving patients with severe protein malnutrition. Comparison of this group with a group of healthy subjects revealed significantly lower GSH concentrations in erythrocytes in the former, thus proving that the described GC-MS method could be employed for fast and simple GSH analysis in clinical studies. Copyright © 2017 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.

Extraction Optimization for Phenolic- and Withanolide-Rich Fractions from Withania somnifera Roots: Identification and Quantification of Withaferin A, 12-Deoxywithastromonolide, and Withanolide A in Plant Materials and Marketed Formulations Using a Reversed-Phase HPLC-Photodiode Array Detection Method.

PubMed

Kumar, Satyanshu; Singh, Raghuraj; Gajbhiye, Narendra; Dhanani, Tushar

2018-06-26

Background : Both the roots and leaves of Withania somnifera are products of commerce. They contain active compounds of therapeutic value and mostly different withanolides. Several pharmacological activities of W. somnifera have links to one or more withanolides. The presence of phenolic compounds in extracts could play a vital role in the reduction of blood glucose levels in diabetic subjects. Objective : The present study was carried out for the selection of a solvent to prepare extracts rich in phenolics, withaferin A (WA), 12-deoxywithastromonolide (12WD), and withanolide A (WDA). A simple, rapid HPLC method was also developed for the identification and quantification of WA, 12WD, and WDA. Methods : The extraction efficiency of aqueous alcoholic solvents including hexane, chloroform, ethyl acetate, and methanol were compared for three selected withanolides and total phenolic content. The contents of WA, 12WD, and WDA and total phenolics were determined in the extracts. The quality of nine formulations containing W. sominfera were also compared in terms of the content of WA, 12WD, and WDA and total phenolics. Results : The maximum extract yield and the total withanolide and phenolic content were obtained from aqueous alcoholic compositions at 50:50 (v/v), 70:30 (v/v), and 100:0 (v/v), respectively. In the case of organic solvents, chloroform and ethyl acetate yielded the highest concentrations of phenolics and three withanolides, respectively. The total phenolic content in formulations was in the range of 1.84-3.13%, and total withanolide content showed wide variability. Conclusions : The outcome of the present investigation could be utilized for the selection of extraction solvents to prepare W. somnifera -enriched extracts and their quality monitoring by using the developed and validated HPLC-Photodiode array detection method. Highlights : A process for preparation of phenolics and withanolides (withaferin A, 12-deoxywithastramonolide and withanolide A) enriched extracts of Withania somnifera . Simple and rapid HPLC method was also developed and validated as per the ICH guidelines for identification and quantification of three major withanolides. The developed HPLC method was applied to analyze the quality of extracts and marketed herbal products (mono, as well as poly constituents). Optimized extraction process could be utilized for upscaling process development in preparation of enriched extracts from Withania somnifera , crop improvement, bio-prospection studies and quality control.

Cloud point extraction and determination of trace trichlorfon by high performance liquid chromatography with ultraviolet-detection based on its catalytic effect on benzidine oxidizing.

PubMed

Zhu, Hai-Zhen; Liu, Wei; Mao, Jian-Wei; Yang, Ming-Min

2008-04-28

4-Amino-4'-nitrobiphenyl, which is formed by catalytic effect of trichlorfon on sodium perborate oxidizing benzidine, is extracted with a cloud point extraction method and then detected using a high performance liquid chromatography with ultraviolet detection (HPLC-UV). Under the optimum experimental conditions, there was a linear relationship between trichlorfon in the concentration range of 0.01-0.2 mgL(-1) and the peak areas of 4-amino-4'-nitrobiphenyl (r=0.996). Limit of detection was 2.0 microgL(-1), recoveries of spiked water and cabbage samples ranged between 95.4-103 and 85.2-91.2%, respectively. It was proved that the cloud point extraction (CPE) method was simple, cheap, and environment friendly than extraction with organic solvents and had more effective extraction yield.

Shape information from glucose curves: Functional data analysis compared with traditional summary measures

PubMed Central

2013-01-01

Background Plasma glucose levels are important measures in medical care and research, and are often obtained from oral glucose tolerance tests (OGTT) with repeated measurements over 2–3 hours. It is common practice to use simple summary measures of OGTT curves. However, different OGTT curves can yield similar summary measures, and information of physiological or clinical interest may be lost. Our mean aim was to extract information inherent in the shape of OGTT glucose curves, compare it with the information from simple summary measures, and explore the clinical usefulness of such information. Methods OGTTs with five glucose measurements over two hours were recorded for 974 healthy pregnant women in their first trimester. For each woman, the five measurements were transformed into smooth OGTT glucose curves by functional data analysis (FDA), a collection of statistical methods developed specifically to analyse curve data. The essential modes of temporal variation between OGTT glucose curves were extracted by functional principal component analysis. The resultant functional principal component (FPC) scores were compared with commonly used simple summary measures: fasting and two-hour (2-h) values, area under the curve (AUC) and simple shape index (2-h minus 90-min values, or 90-min minus 60-min values). Clinical usefulness of FDA was explored by regression analyses of glucose tolerance later in pregnancy. Results Over 99% of the variation between individually fitted curves was expressed in the first three FPCs, interpreted physiologically as “general level” (FPC1), “time to peak” (FPC2) and “oscillations” (FPC3). FPC1 scores correlated strongly with AUC (r=0.999), but less with the other simple summary measures (−0.42≤r≤0.79). FPC2 scores gave shape information not captured by simple summary measures (−0.12≤r≤0.40). FPC2 scores, but not FPC1 nor the simple summary measures, discriminated between women who did and did not develop gestational diabetes later in pregnancy. Conclusions FDA of OGTT glucose curves in early pregnancy extracted shape information that was not identified by commonly used simple summary measures. This information discriminated between women with and without gestational diabetes later in pregnancy. PMID:23327294

The function of digestive enzymes on Cu, Zn, and Pb release from soil in in vitro digestion tests.

PubMed

Li, Yi; Demisie, Walelign; Zhang, Ming-kui

2013-07-01

The bioaccessibility of soil heavy metals is the solubility of soil heavy metals in synthetic human digestive juice, which is usually determined using in vitro digestion test. To reveal the effects of digestive enzymes on soil heavy metals bioaccessibility, three representative in vitro digestion tests, Simple Bioaccessibility Extraction Test (SBET), Physiologically Based Extraction Test (PBET), and Simple Gastrointestinal Extraction Test (SGET), were chosen. The bioaccessibility of soil Cu, Zn, and Pb in each method were respectively evaluated with and without digestive enzymes, and the differences were compared. The results showed that the effects of digestive enzymes varied with different methods and elements. Because of digestive enzymes addition, the environmental change from acid gastric phase to neutral intestinal phase of PBET did not result in apparently decrease of the bioaccessibility of soil Cu. However, the solubility of soil Zn and Pb were pH-dependent. For SGET, when digestive enzymes were added, its results reflected more variations resulting from soil and element types. The impacts of digestive enzymes on heavy metal dissolution are mostly seen in the intestinal phase. Therefore, digestive enzyme addition is indispensable to the gastrointestinal digestion methods (PBET and SGET), while the pepsin addition is not important for the methods only comprised of gastric digestion (SBET).

The loss of essential oil components induced by the Purge Time in the Pressurized Liquid Extraction (PLE) procedure of Cupressus sempervirens.

PubMed

Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota

2012-05-30

The influence of different Purge Times on the effectiveness of Pressurized Liquid Extraction (PLE) of volatile oil components from cypress plant matrix (Cupressus sempervirens) was investigated, applying solvents of diverse extraction efficiencies. The obtained results show the decrease of the mass yields of essential oil components as a result of increased Purge Time. The loss of extracted components depends on the extrahent type - the greatest mass yield loss occurred in the case of non-polar solvents, whereas the smallest was found in polar extracts. Comparisons of the PLE method with Sea Sand Disruption Method (SSDM), Matrix Solid-Phase Dispersion Method (MSPD) and Steam Distillation (SD) were performed to assess the method's accuracy. Independent of the solvent and Purge Time applied in the PLE process, the total mass yield was lower than the one obtained for simple, short and relatively cheap low-temperature matrix disruption procedures - MSPD and SSDM. Thus, in the case of volatile oils analysis, the application of these methods is advisable. Copyright © 2012 Elsevier B.V. All rights reserved.

Extraction of chemical warfare agents from water with hydrophilic-lipophilic balance and C18 cartridges: comparative study.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Dubey, D K

2007-01-19

Efficient extraction of chemical warfare agents (CWAs) from water is essential before subjecting them to gas chromatographic and spectral analysis aiming towards verification of the Chemical Weapons Convention (CWC). It requires development of fast, reliable, simple and reproducible sample preparation of CWAs from water which is likely to be contaminated during deliberate or inadvertent spread of CWAs. This work describes development of a solid-phase extraction method using hydrophilic-lipophilic balance (HLB) cartridges for extraction of CWAs from water. The extraction efficiencies of HLB and C18 cartridges were compared and the results revealed that HLB sorbents performed better. Extracts were analyzed by gas chromatography-mass spectrometry. Extraction parameters, such as extraction solvent, its volume and rinsing solvent were optimized. Best recoveries of target analytes were obtained using 1mL methanol and limits of detection were achieved up to 0.05microg/mL with dichloromethane. Precision of the method was found to be less than 9.2% RSD.

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

PubMed

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of a solid-phase extraction method for determination of pheophorbide a and pyropheophorbide a in health foods by liquid chromatography.

PubMed

Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

2004-01-01

A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1-102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 microg/g and from <1 to 24 microg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid-liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.

Rapid and simple method for the determination of emodin in tartary buckwheat (Fagopyrum tataricum) by high-performance liquid chromatography coupled to a diode array detector.

PubMed

Peng, Lian-Xin; Wang, Jing-Bo; Hu, Li-Xue; Zhao, Jiang-Lin; Xiang, Da-Bing; Zou, Liang; Zhao, Gang

2013-01-30

A simple and rapid method for determining emodin, an active factor presented in tartary buckwheat (Fagopyrum tataricum), by high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD) has been developed. Emodin was separated from an extract of buckwheat on a Kromasil-ODS C(18) (250 mm × 4.6 mm × 5 μm) column. The separation is achieved within 15 min on the ODS column. Emodin can be quantified using an external standard method detecting at 436 nm. Good linearity is obtained with a correlation coefficient exceeding 0.9992. The limit of detection and the limit of quantification are 5.7 and 19 μg/L, respectively. This method shows good reproducibility for the quantification of the emodin with a relative standard deviation value of 4.3%. Under optimized extraction conditions, the recovery of emodin was calculated as >90%. The validated method is successfully applied to quantify the emodin in tartary buckwheat and its products.

Simultaneous extraction, identification and quantification of phenolic compounds in Eclipta prostrata using microwave-assisted extraction combined with HPLC-DAD-ESI-MS/MS.

PubMed

Fang, Xinsheng; Wang, Jianhua; Hao, Jifu; Li, Xueke; Guo, Ning

2015-12-01

A simple and rapid method was developed using microwave-assisted extraction (MAE) combined with HPLC-DAD-ESI-MS/MS for the simultaneous extraction, identification, and quantification of phenolic compounds in Eclipta prostrata, a common herb and vegetable in China. The optimized parameters of MAE were: employing 50% ethanol as solvent, microwave power 400 W, temperature 70 °C, ratio of liquid/solid 30 mL/g and extraction time 2 min. Compared to conventional extraction methods, the optimized MAE can avoid the degradation of the phenolic compounds and simultaneously obtained the highest yields of all components faster with less consumption of solvent and energy. Six phenolic acids, six flavonoid glycosides and one coumarin were firstly identified. The phenolic compounds were quantified by HPLC-DAD with good linearity, precision, and accuracy. The extract obtained by MAE showed significant antioxidant activity. The proposed method provides a valuable and green analytical methodology for the investigation of phenolic components in natural plants. Copyright © 2015 Elsevier Ltd. All rights reserved.

Carrier mediated hollow fiber liquid phase microextraction combined with HPLC-UV for preconcentration and determination of some tetracycline antibiotics.

PubMed

Shariati, Shahab; Yamini, Yadollah; Esrafili, Ali

2009-02-01

In the present study, a simple and efficient preconcentration method was developed using carrier mediated three phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of trace amounts of highly hydrophilic tetracycline antibiotics including tetracycline (TCN), oxytetracycline (OTCN) and doxycycline (DCN) in bovine milk, human plasma and water samples. For extraction, 11.0 mL of the aqueous sample containing TCNs and 0.05 M Na(2)HPO(4) (9.10.995). Finally, applicability of the proposed method was successfully confirmed by extraction and determination of the drugs in water and plasma samples as well as in bovine milk samples with low and high fat contents. Comparing to the traditional methods, the proposed method exhibits high sensitivity and high preconcentration factors as well as good precision. The extraction setup is simple and due to active transport of analytes, high cleanup effect and good selectivity are obtained in extraction process.

Determination of triclosan in antiperspirant gels by first-order derivative spectrophotometry.

PubMed

Du, Lina; Li, Miao; Jin, Yiguang

2011-10-01

A first-order derivative UV spectrophotometric method was developed to determine triclosan, a broad-spectrum antimicrobial agent, in health care products containing fragrances which could interfere the determination as impurities. Different extraction methods were compared. Triclosan was extracted with chloroform and diluted with ethanol followed by the derivative spectrophotometric measurement. The interference of fragrances was completely eliminated. The calibration graph was found to be linear in the range of 7.5-45 microg x mL(-1). The method is simple, rapid, sensitive and proper to determine triclosan in fragrance-containing health care products.

Development of water-phase derivatization followed by solid-phase microextraction and gas chromatography/mass spectrometry for fast determination of valproic acid in human plasma.

PubMed

Deng, Chunhui; Li, Ning; Ji, Jie; Yang, Bei; Duan, Gengli; Zhang, Xiangmin

2006-01-01

In this study, a simple, rapid, and sensitive method was developed and validated for the quantification of valproic acid (VPA), an antiepileptic drug, in human plasma, which was based on water-phase derivatization followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS). In the proposed method, VPA in plasma was rapidly derivatized with a mixture of isobutyl chloroformate, ethanol and pyridine under mild conditions (room temperature, aqueous medium), and the VPA ethyl ester formed was headspace-extracted and simultaneously concentrated using the SPME technique. Finally, the analyte extracted on SPME fiber was analyzed by GC/MS. The experimental parameters and method validations were studied. The optimal conditions were obtained: PDMS fiber, stirring rate of 1100 rpm, sample temperature of 80 degrees C, extraction time of 20 min, NaCl concentration of 30%. The proposed method had a limit of quantification (0.3 microg/mL), good recovery (89-97%) and precision (RSD value less than 10%). Because the proposed method combined a rapid water-phase derivatization with a fast, simple and solvent-free sample extraction and concentration technique of SPME, the sample preparation time was less than 25 min. This much shortens the whole analysis time of VPA in plasma. The validated method has been successfully used to analyze VPA in human plasma samples for application in pharmacokinetic studies. All these results show that water-phase derivatization followed by HS-SPME and GC/MS is an alternative and powerful method for fast determination of VPA in biological fluids. Copyright 2006 John Wiley & Sons, Ltd.

From Sour Grapes to Low-Hanging Fruit: A Case Study Demonstrating a Practical Strategy for Natural Language Processing Portability.

PubMed

Johnson, Stephen B; Adekkanattu, Prakash; Campion, Thomas R; Flory, James; Pathak, Jyotishman; Patterson, Olga V; DuVall, Scott L; Major, Vincent; Aphinyanaphongs, Yindalon

2018-01-01

Natural Language Processing (NLP) holds potential for patient care and clinical research, but a gap exists between promise and reality. While some studies have demonstrated portability of NLP systems across multiple sites, challenges remain. Strategies to mitigate these challenges can strive for complex NLP problems using advanced methods (hard-to-reach fruit), or focus on simple NLP problems using practical methods (low-hanging fruit). This paper investigates a practical strategy for NLP portability using extraction of left ventricular ejection fraction (LVEF) as a use case. We used a tool developed at the Department of Veterans Affair (VA) to extract the LVEF values from free-text echocardiograms in the MIMIC-III database. The approach showed an accuracy of 98.4%, sensitivity of 99.4%, a positive predictive value of 98.7%, and F-score of 99.0%. This experience, in which a simple NLP solution proved highly portable with excellent performance, illustrates the point that simple NLP applications may be easier to disseminate and adapt, and in the short term may prove more useful, than complex applications.

Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography.

PubMed

Tejada-Casado, Carmen; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M; Lara, Francisco J

2018-08-01

A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in <32 min, using a Zorbax XDB-C18 column (150 mm × 0.5 mm I.D, 5 μm), with a mobile phase consisting of 50 mM ammonium acetate (solvent A) and a mixture of acetonitrile/methanol (1:1 v/v) (solvent B), at a flow rate of 9 μL min -1 . The temperature of the column was 20 °C and 6 μL of sample were injected. In spite of the complexity of milk samples, an effective, simple and fast sample preparation method called salting out-assisted liquid-liquid extraction (SALLE) was developed for the analysis of these compounds in cow milk samples. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt. Good linearity was obtained (R 2  > 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg -1 . Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level. Copyright © 2018 Elsevier B.V. All rights reserved.

Comparison of results from simple expressions for MOSFET parameter extraction

NASA Technical Reports Server (NTRS)

Buehler, M. G.; Lin, Y.-S.

1988-01-01

In this paper results are compared from a parameter extraction procedure applied to the linear, saturation, and subthreshold regions for enhancement-mode MOSFETs fabricated in a 3-micron CMOS process. The results indicate that the extracted parameters differ significantly depending on the extraction algorithm and the distribution of I-V data points. It was observed that KP values vary by 30 percent, VT values differ by 50 mV, and Delta L values differ by 1 micron. Thus for acceptance of wafers from foundries and for modeling purposes, the extraction method and data point distribution must be specified. In this paper measurement and extraction procedures that will allow a consistent evaluation of measured parameters are discussed.

Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue.

PubMed

Meyer, Marjolaine D; Terry, Leon A

2008-08-27

Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.

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.

Detection of Chlorogenic Acid in Honeysuckle Using Infrared-Assisted Extraction Followed by Capillary Electrophoresis with UV Detector

PubMed Central

Tang, Zhuxing; Zang, Shuliang; Zhang, Xiangmin

2012-01-01

In this study, a novel infrared-assisted extraction method coupled capillary electrophoresis (CE) is employed to determine chlorogenic acid from a traditional Chinese medicine (TCM), honeysuckle. The effects of pH and the concentration of the running buffer, separation voltage, injection time, IR irradiation time, and anhydrous ethanol in the extraction concentration were investigated. The optimal conditions were as follows: extraction time, 30 min; extraction solvent, 80% (v/v) ethanol in water solution; and 50 mmol/L borate buffer (pH 8.7) was used as the running buffer at a separation voltage of 16 kV. The samples were injected electrokinetically at 16 kV for 8 s. Good linearity (r2 > 0.9996) was observed over the concentration ranges investigated, and the stability of the solutions was high. Recoveries of the chlorogenic acid were from 95.53% to 106.62%, and the relative standard deviation was below 4.1%. By using this novel IR-assisted extraction method, a higher extraction efficiency than those extracted with conventional heat-reflux extraction was found. The developed IR-assisted extraction method is simple, low-cost, and efficient, offering a great promise for the quick determination of active compounds in TCM. The results indicated that IR-assisted extraction followed by CE is a reliable method for quantitative analysis of active ingredient in TCM. PMID:22291060

Authentication of Piper betle L. folium and quantification of their antifungal-activity.

PubMed

Wirasuta, I Made Agus Gelgel; Srinadi, I Gusti Ayu Made; Dwidasmara, Ida Bagus Gede; Ardiyanti, Ni Luh Putu Putri; Trisnadewi, I Gusti Ayu Arya; Paramita, Ni Luh Putu Vidya

2017-07-01

The TLC profiles of intra- and inter-day precision for Piper betle L . (PBL) folium methanol extract was studied for their peak marker recognition and identification. The Numerical chromatographic parameters (NCPs) of the peak markers, the hierarchical clustering analysis (HCA) and the principal component analysis (PCA) were applied to authenticate the PBL. folium extract from other Piper species folium extract and to ensure the antifungal activity quality of the PBL essential oil. The spotted extract was developed with the mobile phase of toluene: ethyl acetate; 93:7, (v/v). The eluted plate was viewed with the TLC-Visualizer, scanned under absorption and fluorescent mode detection, and on each sample the in-situ UV spectra were recorded between 190 to 400 nm. The NCPs profiles of intra- and inter-day precision results offered multi-dimensional chromatogram fingerprints for better marker peak pattern recognition and identification. Using the r -value fingerprints data series generated with this method allowed more precise discrimination the PBL. from other Piper species compared to the marker peak area fingerprint method. The cosine pair comparison was a simple method for authentication of two different fingerprints. The ward linkage clustering and the pair cross-correlation comparison were better chemometric methods to determine the consistency peak area ratio between fingerprints. The first component PCA-loading values of peak marker area fingerprints were correlated linearly to both the bio-marker concentration as well as the antifungal activity. This relationship could be used to control the quality and pharmacological potency. This simple method was developed for the authentication and quantification of herbal medicine.

A simple validated multi-analyte method for detecting drugs in oral fluid by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

PubMed

Zheng, Yufang; Sparve, Erik; Bergström, Mats

2018-06-01

A UPLC-MS/MS method was developed to identify and quantitate 37 commonly abused drugs in oral fluid. Drugs of interest included amphetamines, benzodiazepines, cocaine, opiates, opioids, phencyclidine and tetrahydrocannabinol. Sample preparation and extraction are simple, and analysis times short. Validation showed satisfactory performance at relevant concentrations. The possibility of contaminated samples as well as the interpretation in relation to well-knows matrices, such as urine, will demand further study. Copyright © 2017 John Wiley & Sons, Ltd.

Two-dimensional shape recognition using sparse distributed memory

NASA Technical Reports Server (NTRS)

Kanerva, Pentti; Olshausen, Bruno

1990-01-01

Researchers propose a method for recognizing two-dimensional shapes (hand-drawn characters, for example) with an associative memory. The method consists of two stages: first, the image is preprocessed to extract tangents to the contour of the shape; second, the set of tangents is converted to a long bit string for recognition with sparse distributed memory (SDM). SDM provides a simple, massively parallel architecture for an associative memory. Long bit vectors (256 to 1000 bits, for example) serve as both data and addresses to the memory, and patterns are grouped or classified according to similarity in Hamming distance. At the moment, tangents are extracted in a simple manner by progressively blurring the image and then using a Canny-type edge detector (Canny, 1986) to find edges at each stage of blurring. This results in a grid of tangents. While the technique used for obtaining the tangents is at present rather ad hoc, researchers plan to adopt an existing framework for extracting edge orientation information over a variety of resolutions, such as suggested by Watson (1987, 1983), Marr and Hildreth (1980), or Canny (1986).

Cleanup procedure for water, soil, animal and plant extracts for the use of electron-capture detector in the gas chromatographic analysis of organophosphorus insecticide residues.

PubMed

Kadoum, A M

1968-07-01

A simple, aqueous acetonitrile partition cleanup method for analyses of some common organophosphorus insecticide residues is described. The procedure described is for cleanup and quantitative recovery of parathion, methyl parathion, diazinon, malathion and thimet from different extracts. Those insecticides in the purified extracts of ground water, grain, soil, plant and animal tissues can be detected quantitatively by gas chromatography with an electron capture-detector at 0.01 ppm. Cleanup is satisfactory for paper and thin-layer chromatography for further identification of individual insecticides in the extracts.

Extractive colorimetric method for the determination of dothiepin hydrochloride and risperidone in pure and in dosage forms.

PubMed

Hassan, Wafaa El-Sayed

2008-08-01

Three rapid, simple, reproducible and sensitive extractive colorimetric methods (A--C) for assaying dothiepin hydrochloride (I) and risperidone (II) in bulk sample and in dosage forms were investigated. Methods A and B are based on the formation of an ion pair complexes with methyl orange (A) and orange G (B), whereas method C depends on ternary complex formation between cobalt thiocyanate and the studied drug I or II. The optimum reaction conditions were investigated and it was observed the calibration curves resulting from the measurements of absorbance concentration relations of the extracted complexes were linear over the concentration range 0.1--12 microg ml(-1) for method A, 0.5--11 mug ml(-1) for method B, and 3.2--80 microg ml(-1) for method C with a relative standard deviation (RSD) of 1.17 and 1.28 for drug I and II, respectively. The molar absorptivity, Sandell sensitivity, Ringbom optimum concentration ranges, and detection and quantification limits for all complexes were calculated and evaluated at maximum wavelengths of 423, 498, and 625 nm, using methods A, B, and C, respectively. The interference from excipients commonly present in dosage forms and common degradation products was studied. The proposed methods are highly specific for the determination of drugs I and II, in their dosage forms applying the standard additions technique without any interference from common excipients. The proposed methods have been compared statistically to the reference methods and found to be simple, accurate (t-test) and reproducible (F-value).

Improving performances of suboptimal greedy iterative biclustering heuristics via localization.

PubMed

Erten, Cesim; Sözdinler, Melih

2010-10-15

Biclustering gene expression data is the problem of extracting submatrices of genes and conditions exhibiting significant correlation across both the rows and the columns of a data matrix of expression values. Even the simplest versions of the problem are computationally hard. Most of the proposed solutions therefore employ greedy iterative heuristics that locally optimize a suitably assigned scoring function. We provide a fast and simple pre-processing algorithm called localization that reorders the rows and columns of the input data matrix in such a way as to group correlated entries in small local neighborhoods within the matrix. The proposed localization algorithm takes its roots from effective use of graph-theoretical methods applied to problems exhibiting a similar structure to that of biclustering. In order to evaluate the effectivenesss of the localization pre-processing algorithm, we focus on three representative greedy iterative heuristic methods. We show how the localization pre-processing can be incorporated into each representative algorithm to improve biclustering performance. Furthermore, we propose a simple biclustering algorithm, Random Extraction After Localization (REAL) that randomly extracts submatrices from the localization pre-processed data matrix, eliminates those with low similarity scores, and provides the rest as correlated structures representing biclusters. We compare the proposed localization pre-processing with another pre-processing alternative, non-negative matrix factorization. We show that our fast and simple localization procedure provides similar or even better results than the computationally heavy matrix factorization pre-processing with regards to H-value tests. We next demonstrate that the performances of the three representative greedy iterative heuristic methods improve with localization pre-processing when biological correlations in the form of functional enrichment and PPI verification constitute the main performance criteria. The fact that the random extraction method based on localization REAL performs better than the representative greedy heuristic methods under same criteria also confirms the effectiveness of the suggested pre-processing method. Supplementary material including code implementations in LEDA C++ library, experimental data, and the results are available at http://code.google.com/p/biclustering/ cesim@khas.edu.tr; melihsozdinler@boun.edu.tr Supplementary data are available at Bioinformatics online.

A simple iterative independent component analysis algorithm for vibration source signal identification of complex structures

NASA Astrophysics Data System (ADS)

Lee, Dong-Sup; Cho, Dae-Seung; Kim, Kookhyun; Jeon, Jae-Jin; Jung, Woo-Jin; Kang, Myeng-Hwan; Kim, Jae-Ho

2015-01-01

Independent Component Analysis (ICA), one of the blind source separation methods, can be applied for extracting unknown source signals only from received signals. This is accomplished by finding statistical independence of signal mixtures and has been successfully applied to myriad fields such as medical science, image processing, and numerous others. Nevertheless, there are inherent problems that have been reported when using this technique: instability and invalid ordering of separated signals, particularly when using a conventional ICA technique in vibratory source signal identification of complex structures. In this study, a simple iterative algorithm of the conventional ICA has been proposed to mitigate these problems. The proposed method to extract more stable source signals having valid order includes an iterative and reordering process of extracted mixing matrix to reconstruct finally converged source signals, referring to the magnitudes of correlation coefficients between the intermediately separated signals and the signals measured on or nearby sources. In order to review the problems of the conventional ICA technique and to validate the proposed method, numerical analyses have been carried out for a virtual response model and a 30 m class submarine model. Moreover, in order to investigate applicability of the proposed method to real problem of complex structure, an experiment has been carried out for a scaled submarine mockup. The results show that the proposed method could resolve the inherent problems of a conventional ICA technique.

Determination of Three Corticosteroids in the Biologic Matrix of Vitreous Humor by HPLC-tandem Mass Spectrometry: Method Development and Validation.

PubMed

Prieto, Esther; Vispe, Eugenio; Otín-Mallada, Sofía; Garcia-Martin, Elena; Polo-Llorens, Vicente; Fraile, José M; Pablo, Luis E; Mayoral, José A

2017-02-01

To develop a simple, specific, and rapid method to determine corticosteroid concentrations in vitreous humor. An analytical method based on high-pressure liquid chromatography-tandem mass spectrometry (HPLC-MS) with a simple extraction procedure was developed. New Zealand albino rabbits (n = 54) received a single (0.1 mL) intravitreal injection of dexamethasone (DXM, 0.1 mg), methylprednisolone (MP, 2 mg), or triamcinolone acetonide (TA, 10 mg). Eyes were enucleated and mean vitreous steroid levels were quantified at 12 h and 1, 2, 3, 7, and 14 days. Corticosteroids were extracted from the vitreous with acetonitrile, and TA was extracted with ethyl acetate, yielding high protein precipitation and clean solution samples. Vitreous samples were analyzed by isocratic HPLC-MS with mobile phase comprising acetonitrile and 2 mM ammonium formate buffer in water, pH 3.5. The linear range was 50-100,000 ng/g with a lower quantification limit of 45 ng/g for DXM and MP, and 50 ng/g for TA. Vitreous levels of DXM and MP were not detectable 14 days post-administration. Vitreous levels of TA were positive and stable throughout the study in both injected and control eyes. The HPLC-MS analytical method is an alternative to HPLC-MS/MS methods, sensitive enough for identifying and quantifying steroids in vitreous humor at a therapeutic dosage scale.

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.

Development of a carbon-nanoparticle-coated stirrer for stir bar sorptive extraction by a simple carbon deposition in flame.

PubMed

Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

2016-03-01

Stir bar sorptive extraction is an environmentally friendly microextraction technique based on a stir bar with various sorbents. A commercial stirrer is a good support, but it has not been used in stir bar sorptive extraction due to difficult modification. A stirrer was modified with carbon nanoparticles by a simple carbon deposition process in flame and characterized by scanning electron microscopy and energy-dispersive X-ray spectrometry. A three-dimensional porous coating was formed with carbon nanoparticles. In combination with high-performance liquid chromatography, the stir bar was evaluated using five polycyclic aromatic hydrocarbons as model analytes. Conditions including extraction time and temperature, ionic strength, and desorption solvent were investigated by a factor-by-factor optimization method. The established method exhibited good linearity (0.01-10 μg/L) and low limits of quantification (0.01 μg/L). It was applied to detect model analytes in environmental water samples. No analyte was detected in river water, and five analytes were quantified in rain water. The recoveries of five analytes in two samples with spiked at 2 μg/L were in the range of 92.2-106% and 93.4-108%, respectively. The results indicated that the carbon nanoparticle-coated stirrer was an efficient stir bar for extraction analysis of some polycyclic aromatic hydrocarbons. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

PubMed

Yu, Chunhe; Hu, Bin

2012-02-15

A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Ultrasound-assisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A. Juss. (Meliaceae) and its determination by a validated HPLC-PDA method.

PubMed

de Paula, Joelma Abadia Marciano; Brito, Lucas Ferreira; Caetano, Karen Lorena Ferreira Neves; de Morais Rodrigues, Mariana Cristina; Borges, Leonardo Luiz; da Conceição, Edemilson Cardoso

2016-01-01

Azadirachta indica A. Juss., also known as neem, is a Meliaceae family tree from India. It is globally known for the insecticidal properties of its limonoid tetranortriterpenoid derivatives, such as azadirachtin. This work aimed to optimize the azadirachtin ultrasound-assisted extraction (UAE) and validate the HPLC-PDA analytical method for the measurement of this marker in neem dried fruit extracts. Box-Behnken design and response surface methodology (RSM) were used to investigate the effect of process variables on the UAE. Three independent variables, including ethanol concentration (%, w/w), temperature (°C), and material-to-solvent ratio (gmL(-1)), were studied. The azadirachtin content (µgmL(-1)), i.e., dependent variable, was quantified by the HPLC-PDA analytical method. Isocratic reversed-phase chromatography was performed using acetonitrile/water (40:60), a flow of 1.0mLmin(-1), detection at 214nm, and C18 column (250×4.6mm(2), 5µm). The primary validation parameters were determined according to ICH guidelines and Brazilian legislation. The results demonstrated that the optimal UAE condition was obtained with ethanol concentration range of 75-80% (w/w), temperature of 30°C, and material-to-solvent ratio of 0.55gmL(-1). The HPLC-PDA analytical method proved to be simple, selective, linear, precise, accurate and robust. The experimental values of azadirachtin content under optimal UAE conditions were in good agreement with the RSM predicted values and were superior to the azadirachtin content of percolated extract. Such findings suggest that UAE is a more efficient extractive process in addition to being simple, fast, and inexpensive. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimisation of solid-phase microextraction coupled to HPLC-UV for the determination of organochlorine pesticides and their metabolites in environmental liquid samples.

PubMed

Torres Padrón, M E; Sosa Ferrera, Z; Santana Rodríguez, J J

2006-09-01

A solid-phase microextraction (SPME) procedure using two commercial fibers coupled with high-performance liquid chromatography (HPLC) is presented for the extraction and determination of organochlorine pesticides in water samples. We have evaluated the extraction efficiency of this kind of compound using two different fibers: 60-mum polydimethylsiloxane-divinylbenzene (PDMS-DVB) and Carbowax/TPR-100 (CW/TPR). Parameters involved in the extraction and desorption procedures (e.g. extraction time, ionic strength, extraction temperature, desorption and soaking time) were studied and optimized to achieve the maximum efficiency. Results indicate that both PDMS-DVB and CW/TPR fibers are suitable for the extraction of this type of compound, and a simple calibration curve method based on simple aqueous standards can be used. All the correlation coefficients were better than 0.9950, and the RSDs ranged from 7% to 13% for 60-mum PDMS-DVB fiber and from 3% to 10% for CW/TPR fiber. Optimized procedures were applied to the determination of a mixture of six organochlorine pesticides in environmental liquid samples (sea, sewage and ground waters), employing HPLC with UV-diode array detector.

Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis.

PubMed

Huang, Xiaojia; Lin, Jianbin; Yuan, Dongxing; Hu, Rongzong

2009-04-17

In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%.

Magnetic graphene dispersive solid phase extraction combining high performance liquid chromatography for determination of fluoroquinolones in foods.

PubMed

He, Xin; Wang, Geng Nan; Yang, Kun; Liu, Hui Zhi; Wu, Xia Jun; Wang, Jian Ping

2017-04-15

In this study, a magnetic graphene-based dispersive solid phase extraction method was developed that was combined with high performance liquid chromatography to determine the residues of fluoroquinolone drugs in foods of animal origin. During the experiments, several parameters possible influencing the extraction performance were optimized (amount of magnetic graphene, sample pH, extraction time and elution solution). This extraction method showed high absorption capacities (>6800ng) and high enrichment factors (68-79-fold) for seven fluoroquinolones. Furthermore, this absorbent could be reused for at least 40 times. The limits of detection were in the range of 0.05-0.3ng/g, and the recoveries from the standards fortified blank samples (bovine milk, chicken muscle and egg) were in the range of 82.4-108.5%. Therefore, this method could be used as a simple and sensitive tool to determine the residues of fluoroquinolones in foods of animal origin. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparation of Multiwalled Carbon Nanotubes/Hydroxyl-Terminated Silicone Oil Fiber and Its Application to Analysis of Crude Oils

PubMed Central

Tong, Ting; Zhang, Wanfeng; Dai, Wei; He, Sheng; Chang, Zhenyang; Gao, Xuanbo

2014-01-01

A simple and efficient method to analyze the volatile and semivolatile organic compounds in crude oils has been developed based on direct immersion solid-phase microextraction coupled to comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (DI-SPME-GC × GC/TOFMS). A novel fiber, multiwalled carbon nanotubes/hydroxyl-terminated silicone oil (MWNTs-TSO-OH), was prepared by sol-gel technology. Using standard solutions, the extraction conditions were optimized such as extraction mode, extraction temperature, extraction time, and salts effect. With the optimized conditions, a real crude oil sample was extracted and then analyzed in detail. It shows that the proposed method is very effective in simultaneously analyzing the normal and branched alkanes, cycloalkanes, aromatic hydrocarbons, and biomarkers of crude oil such as steranes and terpanes. Furthermore, the method showed good linearity (r > 0.999), precision (RSD < 8%), and detection limits ranging from 0.2 to 1.6 ng/L. PMID:24578659

Studying DNA in the Classroom.

ERIC Educational Resources Information Center

Zarins, Silja

1993-01-01

Outlines a workshop for teachers that illustrates a method of extracting DNA and provides instructions on how to do some simple work with DNA without sophisticated and expensive equipment. Provides details on viscosity studies and breaking DNA molecules. (DDR)

Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

PubMed

Li, Na; Wu, Lijie; Nian, Li; Song, Ying; Lei, Lei; Yang, Xiao; Wang, Kun; Wang, Zhibing; Zhang, Liyuan; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

2015-09-01

Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Two-step voltage dual electromembrane extraction: A new approach to simultaneous extraction of acidic and basic drugs.

PubMed

Asadi, Sakine; Nojavan, Saeed

2016-06-07

In the present work, acidic and basic drugs were simultaneously extracted by a novel method of high efficiency herein referred to as two-step voltage dual electromembrane extraction (TSV-DEME). Optimizing effective parameters such as composition of organic liquid membrane, pH values of donor and acceptor solutions, voltage and duration of each step, the method had its figures of merit investigated in pure water, human plasma, wastewater, and breast milk samples. Simultaneous extraction of acidic and basic drugs was done by applying potentials of 150 V and 400 V for 6 min and 19 min as the first and second steps, respectively. The model compounds were extracted from 4 mL of sample solution (pH = 6) into 20 μL of each acceptor solution (32 mM NaOH for acidic drugs and 32 mM HCL for basic drugs). 1-Octanol was immobilized within the pores of a porous hollow fiber of polypropylene, as the supported liquid membrane (SLM) for acidic drugs, and 2-ethyle hexanol, as the SLM for basic drugs. The proposed TSV-DEME technique provided good linearity with the resulting correlation coefficients ranging from 0.993 to 0.998 over a concentration range of 1-1000 ng mL(-1). The limit of detections of the drugs were found to range within 0.3-1.5 ng mL(-1), while the corresponding repeatability ranged from 7.7 to 15.5% (n = 4). The proposed method was further compared to simple dual electromembrane extraction (DEME), indicating significantly higher recoveries for TSV-DEME procedure (38.1-68%), as compared to those of simple DEME procedure (17.7-46%). Finally, the optimized TSV-DEME was applied to extract and quantify model compounds in breast milk, wastewater, and plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of a High Intensity Focused Ultrasound-Immobilized Trypsin Digestion and 18O-Labeling Method for Quantitative Proteomics

PubMed Central

López-Ferrer, Daniel; Hixson, Kim K.; Smallwood, Heather; Squier, Thomas C.; Petritis, Konstantinos; Smith, Richard D.

2009-01-01

A new method that uses immobilized trypsin concomitant with ultrasonic irradiation results in ultra-rapid digestion and thorough 18O labeling for quantitative protein comparisons. The reproducible and highly efficient method provided effective digestions in <1 min with a minimized amount of enzyme required compared to traditional methods. This method was demonstrated for digestion of both simple and complex protein mixtures, including bovine serum albumin, a global proteome extract from the bacteria Shewanella oneidensis, and mouse plasma, as well as 18O labeling of such complex protein mixtures, which validated the application of this method for differential proteomic measurements. This approach is simple, reproducible, cost effective, rapid, and thus well-suited for automation. PMID:19555078

Simultaneous Determination of Fluoroquinolones and Sulfonamides Originating from Sewage Sludge Compost

PubMed Central

Herodes, K.

2017-01-01

A simultaneous method for quantitative determination of traces of fluoroquinolones (FQs) and sulfonamides (SAs) in edible plants fertilized with sewage sludge was developed. The compounds were extracted from the plants by rapid and simple liquid extraction followed by extracts clean-up using solid phase extraction. The eluent additive 1,1,1,3,3,3-hexafluoro-2-propanol was used for liquid chromatographic detection to achieve separation of structurally similar antimicrobials like ciprofloxacin and norfloxacin. Identification and quantification of the compounds were performed using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. Method was validated and extraction recoveries of FQs and SAs ranged from 66% to 93%. The limit of quantifications was from 5 ng/g in the case of ofloxacin to 40 ng/g for norfloxacin. The method precision ranged from 1.43% to 2.61%. The developed novel method was used to evaluate the plats antimicrobial uptake (potato (Solanum tuberosum L.), carrot (Daucus carota L.), lettuce (Lactuca sativa L.), and wheat (Triticum vulgare L.)) from soil and migration of the analytes inside the plants. PMID:28695191

The United States Army Medical Department Journal, January - March 2009

DTIC Science & Technology

2009-03-01

and performing routine chemistry testing for moisture, protein, fat , and solids. Chemistry methods range from simple extractions for percent fat ...States and abroad. The risk for food and waterborne disease is greatest in regions with fractured public health and veterinary infrastructure, lack of a...surgery during the deployment. Two aural hematoma repairs, an extraction of an abscessed tooth, and a root canal on a fractured canine tooth were

An Educational Model for Disruption of Bacteria for Protein Studies.

ERIC Educational Resources Information Center

Bhaduri, Saumya; Demchick, Paul H.

1984-01-01

A simple, rapid, and safe method has been developed for disrupting bacterial cells for protein studies. The method involved stepwise treatment of cells with acetone and with sodium dodecyl sulfate solution to allow extraction of cellular proteins for analysis by polyacrylamide gel electrophoresis. Applications for instructional purposes are noted.…

Ion Engine Grid Gap Measurements

NASA Technical Reports Server (NTRS)

Soulas, Gerge C.; Frandina, Michael M.

2004-01-01

A simple technique for measuring the grid gap of an ion engine s ion optics during startup and steady-state operation was demonstrated with beam extraction. The grid gap at the center of the ion optics assembly was measured with a long distance microscope that was focused onto an alumina pin that protruded through the center accelerator grid aperture and was mechanically attached to the screen grid. This measurement technique was successfully applied to a 30 cm titanium ion optics assembly mounted onto an NSTAR engineering model ion engine. The grid gap and each grid s movement during startup from room temperature to both full and low power were measured. The grid gaps with and without beam extraction were found to be significantly different. The grid gaps at the ion optics center were both significantly smaller than the cold grid gap and different at the two power levels examined. To avoid issues associated with a small grid gap during thruster startup with titanium ion optics, a simple method was to operate the thruster initially without beam extraction to heat the ion optics. Another possible method is to apply high voltage to the grids prior to igniting the discharge because power deposition to the grids from the plasma is lower with beam extraction than without. Further testing would be required to confirm this approach.

An Efficient, Simple, and Noninvasive Procedure for Genotyping Aquatic and Nonaquatic Laboratory Animals.

PubMed

Okada, Morihiro; Miller, Thomas C; Roediger, Julia; Shi, Yun-Bo; Schech, Joseph Mat

2017-09-01

Various animal models are indispensible in biomedical research. Increasing awareness and regulations have prompted the adaptation of more humane approaches in the use of laboratory animals. With the development of easier and faster methodologies to generate genetically altered animals, convenient and humane methods to genotype these animals are important for research involving such animals. Here, we report skin swabbing as a simple and noninvasive method for extracting genomic DNA from mice and frogs for genotyping. We show that this method is highly reliable and suitable for both immature and adult animals. Our approach allows a simpler and more humane approach for genotyping vertebrate animals.

[Determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection].

PubMed

Luo, Xiao-Fei; Yang, Yuan; Sun, Cheng-Jun

2012-01-01

To develop a method for the simultaneous determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection. Organophosphorus pesticides in food were extracted ultrasonically with water. Then the extract was cleaned-up with SPE disk and eluted with ethyl acetate. Finally the eluent was condensed to 1mL under N2 at 55 degrees C. Gas chromatography was applied for quantitative detection of the organophosphorus pesticides in the sample. The linear range of the method for all the pesticides were in the range of 0.01-0.5 mg/kg with correlation coefficients of 0.992-1.000. The detection limits of the method were in the range of 0.0005-0.01 mg/kg. The recoveries for most pesticides were 60%-120% with relative standard deviations of less than 15%. The method is simple, sensitive, environmentally friendly and suitable for the determination of organophosphorous pesticides in food.

Flotation of Mineral and Dyes: A Laboratory Experiment for Separation Method Molecular Hitchhikers

ERIC Educational Resources Information Center

Rappon, Tim; Sylvestre, Jarrett A.; Rappon, Manit

2016-01-01

Flotation as a method of separation is widely researched and is applied in many industries. It has been used to address a wide range of environmental issues including treatment of wastewater, recovery of heavy metals for recycling, extraction of minerals in mining, and so forth. This laboratory attempts to show how such a simple method can be used…

Removal of interfering nucleotides from brain extracts containing substance p. Effect of drugs on brain concentrations of substance p

PubMed Central

Laszlo, I.

1963-01-01

Several methods for removing interfering nucleotides, adenosine-5'-monophosphate and adenosine 5'-triphosphate from brain extracts have been studied. An enzymic method, using adenylic acid deaminase, has been found suitable. This deaminates adenosine monophosphate to 5'-inosinic acid, an inactive compound which does not influence the estimations of substance P. Owing to the adenosine triphosphatase content of the enzyme extract, adenosine triphosphate was also inactivated. For the estimation of adenosine monophosphate-deaminase activity, a simple colorimetric method is described which measures the ammonia liberated from adenosine monophosphate. Substance P in mouse brain extracts was estimated after treatment of the animals with various drugs, and after the enzymic removal of interfering nucleotides from the brain extracts. The drugs had no effect on the substance P content of mouse brain. The effect of drugs on the contractions of the guinea-pig ileum induced by substance P was also investigated, and the effect of drugs on the estimations of substance P in brain extracts is discussed. PMID:14066136

Mean centering of ratio spectra and concentration augmented classical least squares in a comparative approach for quantitation of spectrally overlapped bands of antihypertensives in formulations

NASA Astrophysics Data System (ADS)

Hegazy, Maha Abdel Monem; Fayez, Yasmin Mohammed

2015-04-01

Two different methods manipulating spectrophotometric data have been developed, validated and compared. One is capable of removing the signal of any interfering components at the selected wavelength of the component of interest (univariate). The other includes more variables and extracts maximum information to determine the component of interest in the presence of other components (multivariate). The applied methods are smart, simple, accurate, sensitive, precise and capable of determination of spectrally overlapped antihypertensives; hydrochlorothiazide (HCT), irbesartan (IRB) and candesartan (CAN). Mean centering of ratio spectra (MCR) and concentration residual augmented classical least-squares method (CRACLS) were developed and their efficiency was compared. CRACLS is a simple method that is capable of extracting the pure spectral profiles of each component in a mixture. Correlation was calculated between the estimated and pure spectra and was found to be 0.9998, 0.9987 and 0.9992 for HCT, IRB and CAN, respectively. The methods were successfully determined the three components in bulk powder, laboratory-prepared mixtures, and combined dosage forms. The results obtained were compared statistically with each other and to those of the official methods.

A simple and rapid technique for the authentication of the ginseng cultivar, Yunpoong, using an SNP marker in a large sample of ginseng leaves.

PubMed

Sun, Hua; Wang, Hong-Tao; Kwon, Woo-Saeng; Kim, Yeon-Ju; In, Jun-Gyo; Yang, Deok-Chun

2011-11-01

Yunpoong is an important Korean ginseng (Panax ginseng C. A. Meyer) cultivar, but no molecular marker has been available to identify Yunpoong from other cultivars. In this study, we developed a single nucleotide polymorphism (SNP) marker for Yunpoong based on analysis of expressed sequence tags (ESTs) in an exon region of the glyceraldehyde 3-phosphate dehydrogenase (GAPDH) gene. This SNP marker had high specificity to authenticate Yunpoong in twelve different main ginseng cultivars. For application of the molecular marker, a rapid identification method was established based on the NaOH-Tris method and real-time polymerase chain reaction (PCR) in order to ensure more efficiency in the cultivar selection. The biggest feature of the NaOH-Tris method was that it made the extraction of DNA very simple and rapid in young leaf tissues. We only spent 1 min to extract DNA and directly used it to do PCR. In this report, the conventional DNA extraction method was used to develop molecular marker process, and the NaOH-Tris method was applied in screening large numbers of cultivars. Moreover, the greatest advantage of the real-time PCR compared with traditional PCR, is time saving and high efficiency. Thus, this strategy provides a rapid and reliable method for the specific identification of Yunpoong in a large number of samples. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

Using computational modeling of river flow with remotely sensed data to infer channel bathymetry

USGS Publications Warehouse

Nelson, Jonathan M.; McDonald, Richard R.; Kinzel, Paul J.; Shimizu, Y.

2012-01-01

As part of an ongoing investigation into the use of computational river flow and morphodynamic models for the purpose of correcting and extending remotely sensed river datasets, a simple method for inferring channel bathymetry is developed and discussed. The method is based on an inversion of the equations expressing conservation of mass and momentum to develop equations that can be solved for depth given known values of vertically-averaged velocity and water-surface elevation. The ultimate goal of this work is to combine imperfect remotely sensed data on river planform, water-surface elevation and water-surface velocity in order to estimate depth and other physical parameters of river channels. In this paper, the technique is examined using synthetic data sets that are developed directly from the application of forward two-and three-dimensional flow models. These data sets are constrained to satisfy conservation of mass and momentum, unlike typical remotely sensed field data sets. This provides a better understanding of the process and also allows assessment of how simple inaccuracies in remotely sensed estimates might propagate into depth estimates. The technique is applied to three simple cases: First, depth is extracted from a synthetic dataset of vertically averaged velocity and water-surface elevation; second, depth is extracted from the same data set but with a normally-distributed random error added to the water-surface elevation; third, depth is extracted from a synthetic data set for the same river reach using computed water-surface velocities (in place of depth-integrated values) and water-surface elevations. In each case, the extracted depths are compared to the actual measured depths used to construct the synthetic data sets (with two- and three-dimensional flow models). Errors in water-surface elevation and velocity that are very small degrade depth estimates and cannot be recovered. Errors in depth estimates associated with assuming water-surface velocities equal to depth-integrated velocities are substantial, but can be reduced with simple corrections.

Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

PubMed

Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

2017-09-10

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

NASA Astrophysics Data System (ADS)

Zawadowicz, M. A.; Del Negro, L. A.

2010-12-01

Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

Pellet pestle homogenization of agarose gel slices at 45 degrees C for deoxyribonucleic acid extraction.

PubMed

Kurien, B T; Kaufman, K M; Harley, J B; Scofield, R H

2001-09-15

A simple method for extracting DNA from agarose gel slices is described. The extraction is rapid and does not involve harsh chemicals or sophisticated equipment. The method involves homogenization of the excised gel slice (in Tris-EDTA buffer), containing the DNA fragment of interest, at 45 degrees C in a microcentrifuge tube with a Kontes pellet pestle for 1 min. The "homogenate" is then centrifuged for 30 s and the supernatant is saved. The "homogenized" agarose is extracted one more time and the supernatant obtained is combined with the previous supernatant. The DNA extracted using this method lent itself to restriction enzyme analysis, ligation, transformation, and expression of functional protein in bacteria. This method was found to be applicable with 0.8, 1.0, and 2.0% agarose gels. DNA fragments varying from 23 to 0.4 kb were extracted using this procedure and a yield ranging from 40 to 90% was obtained. The yield was higher for fragments 2.0 kb and higher (70-90%). This range of efficiency was maintained when the starting material was kept between 10 and 300 ng. The heat step was found to be critical since homogenization at room temperature failed to yield any DNA. Extracting DNA with our method elicited an increased yield (up to twofold) compared with that extracted with a commercial kit. Also, the number of transformants obtained using the DNA extracted with our method was at least twice that obtained using the DNA extracted with the commercial kit. Copyright 2001 Academic Press.

Optimizing conditions for the extraction of pigments in cochineals (Dactylopius coccus Costa) using response surface methodology.

PubMed

González, Mónica; Méndez, Jesús; Carnero, Aurelio; Lobo, M Gloria; Afonso, Ana

2002-11-20

A simple method was developed for the extraction and determination of color pigments in cochineals (Dactylopius coccus Costa). The procedure was based on the solvent extraction of pigments in insect samples using methanol:water (65:35, v:v) as extractant. Two-level factorial design was used in order to optimize the solvent extraction parameters: temperature, time, methanol concentration in the extractant mixture, and the number of extractions. The results suggest that the number of extractions is statistically the most significant factor. The separation and determination of the pigments was carried out by high-performance liquid chromatography with UV-visible detection. Because the absorption spectra of different pigments are different in the visible region, it is convenient to use a diode array detector to obtain chromatographic profiles that allow for the characterization of the extracted pigments.

Respiratory Artefact Removal in Forced Oscillation Measurements: A Machine Learning Approach.

PubMed

Pham, Thuy T; Thamrin, Cindy; Robinson, Paul D; McEwan, Alistair L; Leong, Philip H W

2017-08-01

Respiratory artefact removal for the forced oscillation technique can be treated as an anomaly detection problem. Manual removal is currently considered the gold standard, but this approach is laborious and subjective. Most existing automated techniques used simple statistics and/or rejected anomalous data points. Unfortunately, simple statistics are insensitive to numerous artefacts, leading to low reproducibility of results. Furthermore, rejecting anomalous data points causes an imbalance between the inspiratory and expiratory contributions. From a machine learning perspective, such methods are unsupervised and can be considered simple feature extraction. We hypothesize that supervised techniques can be used to find improved features that are more discriminative and more highly correlated with the desired output. Features thus found are then used for anomaly detection by applying quartile thresholding, which rejects complete breaths if one of its features is out of range. The thresholds are determined by both saliency and performance metrics rather than qualitative assumptions as in previous works. Feature ranking indicates that our new landmark features are among the highest scoring candidates regardless of age across saliency criteria. F1-scores, receiver operating characteristic, and variability of the mean resistance metrics show that the proposed scheme outperforms previous simple feature extraction approaches. Our subject-independent detector, 1IQR-SU, demonstrated approval rates of 80.6% for adults and 98% for children, higher than existing methods. Our new features are more relevant. Our removal is objective and comparable to the manual method. This is a critical work to automate forced oscillation technique quality control.

Simultaneous estimation of lisofylline and pentoxifylline in rat plasma by high performance liquid chromatography-photodiode array detector and its application to pharmacokinetics in rat.

PubMed

Italiya, Kishan S; Sharma, Saurabh; Kothari, Ishit; Chitkara, Deepak; Mittal, Anupama

2017-09-01

Lisofylline (LSF) is an anti-inflammatory and immunomodulatory agent with proven activity in serious infections associated with cancer chemotherapy, hyperoxia-induced acute lung injury, autoimmune disorders including type-1 diabetes (T1DM) and islet rejection after islet transplantation. It is also an active metabolite of another anti-inflammatory agent, Pentoxifylline (PTX). LSF bears immense therapeutic potential in multiple pharmacological activities and hence appropriate and accurate quantification of LSF is very important. Although a number of analytical methods for quantification of LSF and PTX have been reported for pharmacokinetics and metabolic studies, each of these have certain limitations in terms of large sample volume required, complex extraction procedure and/or use of highly sophisticated instruments like LC-MS/MS. The aim of current study is to develop a simple reversed-phase HPLC method in rat plasma for simultaneous determination of LSF and PTX with the major objective of ensuring minimum sample volume, ease of extraction, economy of analysis, selectivity and avoiding use of instruments like LC-MS/MS to ensure a widespread application of the method. A simple liquid-liquid extraction method using methylene chloride as extracting solvent was used for extracting LSF and PTX from rat plasma (200μL). Samples were then evaporated, reconstituted with mobile phase and injected into HPLC coupled with photo-diode detector (PDA). LSF, PTX and 3-isobutyl 1-methyl xanthine (IBMX, internal standard) were separated on Inertsil® ODS (C18) column (250×4.6mm, 5μm) with mobile phase consisting of A-methanol B-water (50:50v/v) run in isocratic mode at flow rate of 1mL/min for 15min and detection at 273nm. The method showed linearity in the concentration range of 50-5000ng/mL with LOD of 10ng/mL and LLOQ of 50ng/mL for both LSF and PTX. Weighted linear regression analysis was also performed on the calibration data. The mean absolute recoveries were found to be 80.47±3.44 and 80.89±3.73% for LSF and PTX respectively. The method was successfully applied for studying the pharmacokinetics of LSF and PTX after IV bolus administration at dose of 25mg/kg in Wistar rat. In conclusion, a simple, sensitive, accurate and precise reversed-phase HPLC-UV method was established for simultaneous determination of LSF and PTX in rat plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

Non-ionic detergent Triton X-114 Based vortex- synchronized matrix solid-phase dispersion method for the simultaneous determination of six compounds with various polarities from Forsythiae Fructus by ultra high-performance liquid chromatography.

PubMed

Du, Kunze; Li, Jin; Tian, Fei; Chang, Yan-Xu

2018-02-20

A simple nonionic detergent - based vortex- synchronized matrix solid-phase dispersion (ND-VSMSPD) method was developed to extract bioactive compounds in Forsythiae Fructus coupled with ultra high-performance liquid chromatography (UHPLC). Nonionic detergent Triton 114 was firstly used as a green elution reagent in vortex- synchronized MSPD procedure. The optimum parameters were investigated to attain the best results, including Florisil as sorbent, 2mL 10% (v/v) nonionic detergent Triton X-114 as the elution reagent, 1:1 of sample/sorbent ratio, grinding for 3min, and whirling for 2min. The recoveries of the six compounds in Forsythiae Fructus were in the range of 95-104% (RSD <4.6%) and the method displayed a good linearity within the range of 0.08-20μgmL -1 for caffeic acid, 0.6-150μgmL -1 for forsythoside A, 0.4-100μgmL -1 phillyrin, 0.2-50μgmL -1 for quercetin, isorhamnetin and arctigenin (r≥0.999). It was proved that the extraction yields of almost all compounds attained by the established vortex- synchronized MSPD, which required lower sample, reagent and time, were higher than the normal MSPD and the traditional ultrasonic-assisted extraction. Consequently, this developed vortex- synchronized MSPD coupled with simple UHPLC method could be efficiently applies to extract and analyze the target compounds in real Forsythiae Fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Densitometric HPTLC analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams

PubMed Central

Alam, Prawez

2013-01-01

Objective To develop and validate a simple, accurate HPTLC method for the analysis of 8-gingerol and to determine the quantity of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams. Methods The analysis was performed on 10×20 cm aluminium-backed plates coated with 0.2 mm layers of silica gel 60 F254 (E-Merck, Germany) with n-hexane: ethyl acetate 60: 40 (v/v) as mobile phase. Camag TLC Scanner III was used for the UV densitometric scanning at 569. Results This system was found to give a compact spot of 8-gingerol at retention factor (Rf) value of (0.39±0.04) and linearity was found in the ranges 50-500 ng/spot (r2=0.9987). Limit of detection (12.76 ng/spot), limit of quantification (26.32 ng/spot), accuracy (less than 2 %) and recovery (ranging from 98.22-99.20) were found satisfactory. Conclusions The HPTLC method developed for quantification of 8-gingerol was found to be simple, accurate, reproducible, sensitive and is applicable to the analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams. PMID:23905021

Evaluation of Phytoavailability of Heavy Metals to Chinese Cabbage (Brassica chinensis L.) in Rural Soils

PubMed Central

Hseu, Zeng-Yei; Zehetner, Franz

2014-01-01

This study compared the extractability of Cd, Cu, Ni, Pb, and Zn by 8 extraction protocols for 22 representative rural soils in Taiwan and correlated the extractable amounts of the metals with their uptake by Chinese cabbage for developing an empirical model to predict metal phytoavailability based on soil properties. Chemical agents in these protocols included dilute acids, neutral salts, and chelating agents, in addition to water and the Rhizon soil solution sampler. The highest concentrations of extractable metals were observed in the HCl extraction and the lowest in the Rhizon sampling method. The linear correlation coefficients between extractable metals in soil pools and metals in shoots were higher than those in roots. Correlations between extractable metal concentrations and soil properties were variable; soil pH, clay content, total metal content, and extractable metal concentration were considered together to simulate their combined effects on crop uptake by an empirical model. This combination improved the correlations to different extents for different extraction methods, particularly for Pb, for which the extractable amounts with any extraction protocol did not correlate with crop uptake by simple correlation analysis. PMID:25295297

A novel sorptive extraction method based on polydimethylsiloxane frit for determination of lung cancer biomarkers in human serum.

PubMed

Xu, Hui; Wang, Shuyu

2012-04-29

In this study, a porous polypropylene frit was coated with polydimethylsiloxane (PDMS) as extraction medium, based on the home-made PDMS-frit, a rapid, simple and sensitive sorptive extraction method was established for analysis of potential biomarkers of lung cancer (hexanal and heptanal) in human serum samples. In the method, derivatization and extraction occurred simultaneously on the PDMS-frit, then the loaded frit was ultrasonically desorbed in acetonitrile. Polymerization, derivatization-extraction and desorption conditions were optimized. Under the optimal conditions, satisfactory results were gained, a wide linear application range was obtained in the range of 0.002-5.0 μmol L(-1) (R>0.997) for two aldehydes, the detection limits (SN(-1)=3) were 0.5 nmol L(-1) for hexanal and 0.4 nmol L(-1) for heptanal. The relative standard deviations (RSDs, n=5) of the method were below 7.9% and the recoveries were above 72.7% for the spiked serum. All these results hint that the proposed method is potential for disease markers analysis in complex biological samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Effects of different extraction methods on total phenolic content and antioxidant activity in soybean cultivars

NASA Astrophysics Data System (ADS)

Yusnawan, E.

2018-01-01

Soybean secondary metabolites particularly phenolic compounds act as chemical defence against biotic stress such as pathogen infection. Functional properties of these compounds have also been investigated. This study aimed to determine the effects of particle size and extraction methods on total flavonoid, phenolic contents as well as antioxidant activity in soybean seeds. This study also investigated the total phenolic contents and antioxidant activity of Indonesian soybean cultivars using the optimized extraction method. Soybean flour of ≤ 177 μm as many as 0.5 g was selected for extraction with 50% acetone for estimation of total phenolic and flavonoid contents and with 80% ethanol for antioxidant activity. Treatments of twice extraction either shaking followed by maceration or ultrasound-assisted extraction followed by maceration could be used to extract the secondary metabolite contents in soybean seeds. Flavonoid, phenolic contents and antioxidant activity of twenty soybean cultivars ranged from 0.23 to 0.44 mg CE/g, from 3.70 to 5.22 mg GAE/g, and from 4.97 to 9.04 µmol TE/g, respectively. A simple extraction with small amount of soybean flour such as investigated in this present study is effective to extract secondary metabolites especially when the availability of samples is limited such as breeding materials or soybean germplasm.

Combination of solid-phase extraction with dispersive liquid-liquid microextraction followed by GC-MS for determination of pesticide residues from water, milk, honey and fruit juice.

PubMed

Shamsipur, Mojtaba; Yazdanfar, Najmeh; Ghambarian, Mahnaz

2016-08-01

In this work, an effective preconcentration method for the extraction and determination of traces of multi-residue pesticides was developed using solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry (GC-MS). Variables affecting the performance of both extraction steps such as type and volume of elution and extraction solvents, breakthrough volume, salt addition, extraction time were thoroughly investigated. The proposed method resulted in good linearities (R(2)>0.9915) over the ranges of 1-10,000ngkg(-1), limits of detection (LODs) in the range of 0.5-1.0ngkg(-1) at S/N=3, and precision of RSD% of ⩽11.8. Under optimal conditions, the preconcentration factors were obtained in the range of 2362-10,593 for 100mL sample solutions. Comparison of the proposed method with other ones demonstrated that SPE-DLLME method provides higher extraction efficiency and larger preconcentration factor for determination of pesticides residues. Further, it is simple, inexpensive, highly sensitive, and can be successfully applied to separation, preconcentration and determination of the pesticides (and other noxious materials) in different real food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Monitoring of multiple bacteriocins through a developed dual extraction protocol and comparison of HPLC-DAD with turbidometry as their quantification system.

PubMed

Katharopoulos, Efstathios; Touloupi, Katerina; Touraki, Maria

2016-08-01

The present study describes the development of a simple and efficient screening system that allows identification and quantification of nine bacteriocins produced by Lactococcus lactis. Cell-free L. lactis extracts presented a broad spectrum of antibacterial activity, including Gram-negative bacteria, Gram-positive bacteria, and fungi. The characterization of their sensitivity to pH, and heat, showed that the extracts retained their antibacterial activity at extreme pH values and in a wide temperature range. The loss of antibacterial activity following treatment of the extracts with lipase or protease suggests a lipoproteinaceous nature of the produced antimicrobials. The extracts were subjected to a purification protocol that employs a two phase extraction using ammonium sulfate precipitation and organic solvent precipitation, followed by ion exchange chromatography, solid phase extraction and HPLC. In the nine fractions that presented antimicrobial activity, bacteriocins were quantified by the turbidometric method using a standard curve of nisin and by the HPLC method with nisin as the external standard, with both methods producing comparable results. Turbidometry appears to be unique in the qualitative determination of bacteriocins but the only method suitable to both separate and quantify the bacteriocins providing increased sensitivity, accuracy, and precision is HPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

Microwave-assisted extraction at atmospheric pressure coupled to different clean-up methods for the determination of organophosphorus pesticides in olive and avocado oil.

PubMed

Fuentes, Edwar; Báez, María E; Díaz, Juan

2009-12-18

An effective extraction method was devised for the determination of organophosphorus pesticides (OPPs) in olive and avocado oil samples, using atmospheric pressure microwave-assisted liquid-liquid extraction (APMAE) and solid-phase extraction or low-temperature precipitation as clean-up step. A simple glass system equipped with an air-cooled condenser was designed as an extraction vessel. The pesticides were partitioned between acetonitrile and oil solution in hexane. Analytical determinations were carried out by gas chromatography-flame photometric detection and gas chromatography-tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmation purposes. Several factors influencing the extraction efficiency were investigated and optimized through fractional factorial design and Doehlert design. Under optimal conditions the recovery of pesticides from oil at 0.025 microg g(-1) ranged from 71% to 103%, except for fenthion in avocado oil, with RSDs < or = 13% (n=5). The LOQ for the entire method ranged from 0.004 to 0.015 microg g(-1). Finally, the proposed method was successfully applied to the extraction and determination of the selected pesticides in 20 commercially packed extra virgin olive oils and four commercially packed avocado oils produced in Chile. Detectable residues of different OPPs were observed in 85% of samples.

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

PubMed

Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba; Pirsaheb, Meghdad

2013-11-01

A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.

Sensing cocaine in saliva with attenuated total reflection infrared (ATR-IR) spectroscopy combined with a one-step extraction method

NASA Astrophysics Data System (ADS)

Hans, Kerstin M.-C.; Gianella, Michele; Sigrist, Markus W.

2012-03-01

On-site drug tests have gained importance, e.g., for protecting the society from impaired drivers. Since today's drug tests are majorly only positive/negative, there is a great need for a reliable, portable and preferentially quantitative drug test. In the project IrSens we aim to bridge this gap with the development of an optical sensor platform based on infrared spectroscopy and focus on cocaine detection in saliva. We combine a one-step extraction method, a sample drying technique and infrared attenuated total reflection (ATR) spectroscopy. As a first step we have developed an extraction technique that allows us to extract cocaine from saliva to an almost infrared-transparent solvent and to record ATR spectra with a commercially available Fourier Transform-infrared spectrometer. To the best of our knowledge this is the first time that such a simple and easy-to-use one-step extraction method is used to transfer cocaine from saliva into an organic solvent and detect it quantitatively. With this new method we are able to reach a current limit of detection around 10 μg/ml. This new extraction method could also be applied to waste water monitoring and controlling caffeine content in beverages.

Simple and rapid method for the detection of Filobasidiella neoformans in a probiotic dairy product by using loop-mediated isothermal amplification.

PubMed

Ishikawa, Hiroshi; Kasahara, Kohei; Sato, Sumie; Shimakawa, Yasuhisa; Watanabe, Koichi

2014-05-16

Yeast contamination is a serious problem in the food industry and a major cause of food spoilage. Several yeasts, such as Filobasidiella neoformans, which cause cryptococcosis in humans, are also opportunistic pathogens, so a simple and rapid method for monitoring yeast contamination in food is essential. Here, we developed a simple and rapid method that utilizes loop-mediated isothermal amplification (LAMP) for the detection of F. neoformans. A set of five specific LAMP primers was designed that targeted the 5.8S-26S rDNA internal transcribed spacer 2 region of F. neoformans, and the primer set's specificity was confirmed. In a pure culture of F. neoformans, the LAMP assay had a lower sensitivity threshold of 10(2)cells/mL at a runtime of 60min. In a probiotic dairy product artificially contaminated with F. neoformans, the LAMP assay also had a lower sensitivity threshold of 10(2)cells/mL, which was comparable to the sensitivity of a quantitative PCR (qPCR) assay. We also developed a simple two-step method for the extraction of DNA from a probiotic dairy product that can be performed within 15min. This method involves initial protease treatment of the test sample at 45°C for 3min followed by boiling at 100°C for 5min under alkaline conditions. In a probiotic dairy product artificially contaminated with F. neoformans, analysis by means of our novel DNA extraction method followed by LAMP with our specific primer set had a lower sensitivity threshold of 10(3)cells/mL at a runtime of 60min. In contrast, use of our novel method of DNA extraction followed by qPCR assay had a lower sensitivity threshold of only 10(5)cells/mL at a runtime of 3 to 4h. Therefore, unlike the PCR assay, our LAMP assay can be used to quickly evaluate yeast contamination and is sensitive even for crude samples containing bacteria or background impurities. Our study provides a powerful tool for the primary screening of large numbers of food samples for yeast contamination. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparison of Boiling and Robotics Automation Method in DNA Extraction for Metagenomic Sequencing of Human Oral Microbes.

PubMed

Yamagishi, Junya; Sato, Yukuto; Shinozaki, Natsuko; Ye, Bin; Tsuboi, Akito; Nagasaki, Masao; Yamashita, Riu

2016-01-01

The rapid improvement of next-generation sequencing performance now enables us to analyze huge sample sets with more than ten thousand specimens. However, DNA extraction can still be a limiting step in such metagenomic approaches. In this study, we analyzed human oral microbes to compare the performance of three DNA extraction methods: PowerSoil (a method widely used in this field), QIAsymphony (a robotics method), and a simple boiling method. Dental plaque was initially collected from three volunteers in the pilot study and then expanded to 12 volunteers in the follow-up study. Bacterial flora was estimated by sequencing the V4 region of 16S rRNA following species-level profiling. Our results indicate that the efficiency of PowerSoil and QIAsymphony was comparable to the boiling method. Therefore, the boiling method may be a promising alternative because of its simplicity, cost effectiveness, and short handling time. Moreover, this method was reliable for estimating bacterial species and could be used in the future to examine the correlation between oral flora and health status. Despite this, differences in the efficiency of DNA extraction for various bacterial species were observed among the three methods. Based on these findings, there is no "gold standard" for DNA extraction. In future, we suggest that the DNA extraction method should be selected on a case-by-case basis considering the aims and specimens of the study.

A Modified Method for Isolation of Rhein from Senna

PubMed Central

Mehta, Namita; Laddha, K. S.

2009-01-01

A simple and efficient method for the isolation of rhein from Cassia angustifolia (senna) leaves is described in which the hydrolysis of the sennosides and extraction of the hydrolysis products (free anthraquinones) is carried out in one step. Further isolation of rhein is achieved from the anthraquinone mixture. This method reduces the number of steps required for isolation of rhein as compared to conventional methods. PMID:20336207

An efficient method for purifying high quality RNA from wheat pistils.

PubMed

Manickavelu, A; Kambara, Kumiko; Mishina, Kohei; Koba, Takato

2007-02-15

Many methods are available for total RNA extraction from plants, except the floral organs like wheat pistils containing high levels of polysaccharides that bind/or co-precipitate with RNA. In this protocol, a simple and effective method for extracting total RNA from small and feathery wheat pistils has been developed. Lithium chloride (LiCl) and phenol:chloroform:isoamylalcohol (PCI) were employed and the samples were ground in microcentrifuge tube using plastic pestle. A jacket of liquid nitrogen and simplified procedures were applied to ensure thorough grinding of the pistils and to minimize the samples loss. These measures substantially increased the recovery of total RNA (approximately 50%) in the extraction process. Reliable differential display by cDNA-AFLP was successfully achieved with the total RNA after DNase treatment and reverse transcription. This method is also practicable for gene expression and gene regulation studies in floral parts of other plants.

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Kumar, Deenadayalan Ashok; Palanichamy, V.; Roopan, Selvaraj Mohana

2014-06-01

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10 min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis.

General method of pattern classification using the two-domain theory

NASA Technical Reports Server (NTRS)

Rorvig, Mark E. (Inventor)

1993-01-01

Human beings judge patterns (such as images) by complex mental processes, some of which may not be known, while computing machines extract features. By representing the human judgements with simple measurements and reducing them and the machine extracted features to a common metric space and fitting them by regression, the judgements of human experts rendered on a sample of patterns may be imposed on a pattern population to provide automatic classification.

General method of pattern classification using the two-domain theory

NASA Technical Reports Server (NTRS)

Rorvig, Mark E. (Inventor)

1990-01-01

Human beings judge patterns (such as images) by complex mental processes, some of which may not be known, while computing machines extract features. By representing the human judgements with simple measurements and reducing them and the machine extracted features to a common metric space and fitting them by regression, the judgements of human experts rendered on a sample of patterns may be imposed on a pattern population to provide automatic classification.

A Simple and Quick Method for the Determination of Pesticides in Environmental Water by HF-LPME-GC/MS.

PubMed

Menezes, Helvécio C; Paulo, Breno P; Paiva, Maria José N; Cardeal, Zenilda L

2016-01-01

This paper describes a simple and quick method for sampling and also for carrying out the preconcentration of pesticides in environmental water matrices using two-phased hollow fiber liquid phase microextraction (HF-LPME). Factors such as extraction mode, time, solvents, agitation, and salt addition were investigated in order to validate the LPME method. The following conditions were selected: 6 cm of polypropylene hollow fiber, ethyl octanoate as an acceptor phase, and extraction during 30 min under stirring at 200 rpm. The optimized method showed good linearity in the range of 0.14 to 200.00  μ g L -1 ; the determination coefficient ( R 2 ) was in the range of 0.9807-0.9990. The LOD ranged from 0.04  μ g L -1 to 0.44  μ g L -1 , and LOQ ranged from 0.14  μ g L -1 to 1.69  μ g L -1 . The recovery ranged from 85.17% to 114.73%. The method was applied to the analyses of pesticides in three environmental water samples (a spring and few streams) collected in a rural area from the state of Minas Gerais, Brazil.

Noncontact methods for measuring water-surface elevations and velocities in rivers: Implications for depth and discharge extraction

USGS Publications Warehouse

Nelson, Jonathan M.; Kinzel, Paul J.; McDonald, Richard R.; Schmeeckle, Mark

2016-01-01

Recently developed optical and videographic methods for measuring water-surface properties in a noninvasive manner hold great promise for extracting river hydraulic and bathymetric information. This paper describes such a technique, concentrating on the method of infrared videog- raphy for measuring surface velocities and both acoustic (laboratory-based) and laser-scanning (field-based) techniques for measuring water-surface elevations. In ideal laboratory situations with simple flows, appropriate spatial and temporal averaging results in accurate water-surface elevations and water-surface velocities. In test cases, this accuracy is sufficient to allow direct inversion of the governing equations of motion to produce estimates of depth and discharge. Unlike other optical techniques for determining local depth that rely on transmissivity of the water column (bathymetric lidar, multi/hyperspectral correlation), this method uses only water-surface information, so even deep and/or turbid flows can be investigated. However, significant errors arise in areas of nonhydrostatic spatial accelerations, such as those associated with flow over bedforms or other relatively steep obstacles. Using laboratory measurements for test cases, the cause of these errors is examined and both a simple semi-empirical method and computational results are presented that can potentially reduce bathymetric inversion errors.

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.

Simplified multiple headspace extraction gas chromatographic technique for determination of monomer solubility in water.

PubMed

Chai, X S; Schork, F J; DeCinque, Anthony

2005-04-08

This paper reports an improved headspace gas chromatographic (GC) technique for determination of monomer solubilities in water. The method is based on a multiple headspace extraction GC technique developed previously [X.S. Chai, Q.X. Hou, F.J. Schork, J. Appl. Polym. Sci., in press], but with the major modification in the method calibration technique. As a result, only a few iterations of headspace extraction and GC measurement are required, which avoids the "exhaustive" headspace extraction, and thus the experimental time for each analysis. For highly insoluble monomers, effort must be made to minimize adsorption in the headspace sampling channel, transportation conduit and capillary column by using higher operating temperature and a short capillary column in the headspace sampler and GC system. For highly water soluble monomers, a new calibration method is proposed. The combinations of these technique modifications results in a method that is simple, rapid and automated. While the current focus of the authors is on the determination of monomer solubility in aqueous solutions, the method should be applicable to determination of solubility of any organic in water.

Graphene oxide-coated stir bar sorptive extraction of trace aflatoxins from soy milk followed by high performance liquid chromatography-laser-induced fluorescence detection.

PubMed

Ma, Haiyan; Ran, Congcong; Li, Mengjiao; Gao, Jinglin; Wang, Xinyu; Zhang, Lina; Bian, Jing; Li, Junmei; Jiang, Ye

2018-04-01

Mycotoxins are potential food pollutants produced by fungi. Among them, aflatoxins (AFs) are the most toxic. Therefore, AFs were selected as models, and a sensitive, simple and green graphene oxide (GO)-based stir bar sorptive extraction (SBSE) method was developed for extraction and determination of AFs with high performance liquid chromatography-laser-induced fluorescence detector (HPLC-LIF). This method improved the sensitivity of AFs detection and solved the deposition difficulty of the direct use of GO as adsorbent. Several parameters including a spiked amount of NaCl, stirring rate, extraction time and desorption time were investigated. Under optimal conditions, the quantitative method had low limits of detection of 2.4-8.0 pg/mL, which were better than some reported AFs analytical methods. The developed method has been applied to soy milk samples with good recoveries ranging from 80.5 to 102.3%. The prepared GO-based SBSE can be used as a sensitive screening technique for detecting AFs in soy milk.

[Extraction of 10-Deacetyl Baccatin by Supercritical CO2 from Taxus yunnanensis Branches and Leaves].

PubMed

Tang, Yang-qin; Li, Hai-chi; Huang, Wen-jie; Xiong, Yan; Ge, Fa-huan

2015-04-01

To study the supercritical CO2 fluids extraction (SFE) method to extract the components from Taxus yunnanensis. Medicinal meterials were extracted by supercritical CO2, and then purified by industrial chromatography. Using the extraction yield of 10-DAB as the index,single factor test was carried out to investigate the effect of co-solvent, extraction time, extraction pressure, extraction temperature, pressure and temperature of separation kettle I. Then orthogonal experiment was used to optimize the best extraction condition. The suitable extraction condition was as follows: the ratio of co-solvent (80% ethanol) amount and the madicinal materials was 3: 1, Separation kettle I pressure was 14 MPa, separation kettle I temperature was 40 °C, extraction pressure was 25 MPa, extraction temperature was 60 T and extraction time was 90 min. The extract was separated by industrial chromatographic and then crystallized. The supercritical CO2 extraction and purification process of 10-DAB were simple and feasible.

Identification of research hypotheses and new knowledge from scientific literature.

PubMed

Shardlow, Matthew; Batista-Navarro, Riza; Thompson, Paul; Nawaz, Raheel; McNaught, John; Ananiadou, Sophia

2018-06-25

Text mining (TM) methods have been used extensively to extract relations and events from the literature. In addition, TM techniques have been used to extract various types or dimensions of interpretative information, known as Meta-Knowledge (MK), from the context of relations and events, e.g. negation, speculation, certainty and knowledge type. However, most existing methods have focussed on the extraction of individual dimensions of MK, without investigating how they can be combined to obtain even richer contextual information. In this paper, we describe a novel, supervised method to extract new MK dimensions that encode Research Hypotheses (an author's intended knowledge gain) and New Knowledge (an author's findings). The method incorporates various features, including a combination of simple MK dimensions. We identify previously explored dimensions and then use a random forest to combine these with linguistic features into a classification model. To facilitate evaluation of the model, we have enriched two existing corpora annotated with relations and events, i.e., a subset of the GENIA-MK corpus and the EU-ADR corpus, by adding attributes to encode whether each relation or event corresponds to Research Hypothesis or New Knowledge. In the GENIA-MK corpus, these new attributes complement simpler MK dimensions that had previously been annotated. We show that our approach is able to assign different types of MK dimensions to relations and events with a high degree of accuracy. Firstly, our method is able to improve upon the previously reported state of the art performance for an existing dimension, i.e., Knowledge Type. Secondly, we also demonstrate high F1-score in predicting the new dimensions of Research Hypothesis (GENIA: 0.914, EU-ADR 0.802) and New Knowledge (GENIA: 0.829, EU-ADR 0.836). We have presented a novel approach for predicting New Knowledge and Research Hypothesis, which combines simple MK dimensions to achieve high F1-scores. The extraction of such information is valuable for a number of practical TM applications.

Rapid determination of triclosan in personal care products using new in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction coupled with high performance liquid chromatography-ultraviolet detection.

PubMed

Chen, Ming-Jen; Liu, Ya-Ting; Lin, Chiao-Wen; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2013-03-12

This paper describes the development of a novel, simple and efficient in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction (IT-USA-SI-LLME) technique for the rapid determination of triclosan (TCS) in personal care products by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. IT-USA-SI-LLME method is based on the rapid phase separation of water-miscible organic solvent from the aqueous phase in the presence of high concentration of salt (salting-out phenomena) under ultrasonication. In the present work, an indigenously fabricated home-made glass extraction device (8-mL glass tube inbuilt with a self-scaled capillary tip) was utilized as the phase separation device for USA-SI-LLME. After the extraction, the upper extractant layer was narrowed into the self-scaled capillary tip by pushing the plunger plug; thus, the collection and measurement of the upper organic solvent layer was simple and convenient. The effects of various parameters on the extraction efficiency were thoroughly evaluated and optimized. Under optimal conditions, detection was linear in the concentration range of 0.4-100ngmL(-1) with correlation coefficient of 0.9968. The limit of detection was 0.09ngmL(-1) and the relative standard deviations ranged between 0.8 and 5.3% (n=5). The applicability of the developed method was demonstrated for the analysis of TCS in different commercial personal care products and the relative recoveries ranged from 90.4 to 98.5%. The present method was proven to be a simple, sensitive, less organic solvent consuming, inexpensive and rapid procedure for analysis of TCS in a variety of commercially available personal care products or cosmetic preparations. Copyright © 2013 Elsevier B.V. All rights reserved.

Sensitive radioimmunoassay of total thyroxine (T4) in horses using a simple extraction method.

PubMed

Tangyuenyong, Siriwan; Nambo, Yasuo; Nagaoka, Kentaro; Tanaka, Tomomi; Watanabe, Gen

2017-07-28

Most thyroid hormone determinations in animals are based on immunoassays adapted from those used to test human samples, which may not reflect the actual values of thyroid hormone in horses because of the presence of binding proteins. The aims of the present study were i) to establish a novel radioimmunoassay (RIA) using a more simple and convenient method to separate binding proteins for the measurement of total thyroxine (T4) in horses and ii) to validate the assay by comparing total T4 concentrations in yearling horses raised in different climates. Blood samples were collected from trained yearlings in Hokkaido (temperate climate) and Miyazaki (subtropical climate) in Japan and from adult horses in estrus and diestrus. T4 was extracted from both serum and plasma using modified acid ethanol cryo-precipitation and sodium acetate ethanol methods. Circulating total T4 concentrations were determined by RIA. T4 concentration by sodium acetate ethanol was appropriately detectable rather than sodium salicylate method and was the same as for acid ethanol method. Furthermore, this sodium acetate ethanol method required fewer extraction steps than the other methods. Circulating T4 concentrations in yearlings were 225.98 ± 20.89 ng/ml, which was higher than the previous reference values. With respect to climate, T4 levels in Hokkaido yearlings tended to be higher than those in Miyazaki yearlings throughout the study period. These results indicated that this RIA protocol using a modified sodium acetate ethanol separation technique might be an appropriate tool for specific measurement of total T4 in horses.

Development and validation of an analytical method for the separation and determination of major bioactive curcuminoids in Curcuma longa rhizomes and herbal products using non-aqueous capillary electrophoresis.

PubMed

Anubala, S; Sekar, R; Nagaiah, K

2014-06-01

A simple, fast and efficient non-aqueous capillary electrophoresis method (NACE) was developed for the simultaneous determination of three major bioactive curcuminoids (CMNs) in Curcuma longa rhizomes and its herbal products. Good separation, resolution and reproducibility were achieved with the background electrolyte (BGE) consisting a mixture of 15.0 mM sodium tetraborate and 7.4 mM sodium hydroxide (NaOH) in 2:10:15 (v/v/v) of water, 1-propanol, and methanol. The influences of background electrolyte, sodium hydroxide, water, sodium dodecyl sulfate and hydroxylpropyl-β-cyclodextrin on separations were investigated. The separation was carried out in a fused-silica capillary tube with reverse polarity. Hydrodynamic injection of 25mbar for 12s was used for injecting samples and a voltage of 28 kV was applied for separation. The ultrasonication method was used for the extraction of CMNs from the turmeric herbal products and the extract was filtered and directly injected without any further treatments. The limits of detection and quantification were less than 5.0 and 14.6 µg/ml respectively for all CMNs. The percentage recoveries for CMNs were >97.2% (%RSD, <2.62). The results obtained by the method were compared with existing spectrophotometric and HPLC methods. The related compounds in the extract did not interfere in the determination of CMNs. The proposed NACE method is better than existing chromatographic and electrophoretic methods in terms of simple electrophoretic medium, fast analysis and good resolution. Copyright © 2014 Elsevier B.V. All rights reserved.

A simple method for isolation and purification of DIBOA-Glc from Tripsacum dactyloides.

PubMed

Willett, Cammy D; Lerch, Robert N; Goyne, Keith W; Leigh, Nathan D; Lin, Chung-Ho; Roberts, Craig A

2014-09-01

Naturally occurring benzoxazinones (Bx) are a highly reactive class of compounds that have received particular attention in the past several decades. Recently, we identified 2-β-D-glucopyranosyloxy-4-hydroxy-1,4-benzoxazin-3-one (DIBOA-Glc) as the compound present in the roots of Eastern gamagrass {Tripsacum dactyloides (L.)} responsible for atrazine degradation. However, characterization of the DIBOA-Glc/atrazine degradation reaction has been limited due to difficulties in attaining sufficient quantities of purified DIBOA-Glc. The objective of the study was to develop a simple purification and isolation method for obtaining bulk quantities of highly purified DIBOA-Glc. T. dactyloides roots were extracted with 90% aqueous methanol, and the crude extract was fractionated using an HPLC equipped with a C8 semi-prep column and fraction collector. UHPLC-DAD-MS/MS was used to confirm the identity of DIBOA-Glc in the fractions collected. Analysis by 13C and 1H NMR and DAD indicated that 542 mg of DIBOA-Glc with a purity of > 99% was obtained. The reactivity of the DIBOA-Glc was confirmed in a 16 hour assay with atrazine, which resulted in 48.5% ± 1.2% (SD) atrazine degradation. The method described here offers several advantages over existing extraction and synthesis methods, which are more cumbersome, use hazardous chemicals, and yield only small quantities of purified compound. The newly developed method will facilitate future research characterizing the chemical behavior of DIBOA-Glc and determine its potential as an atrazine mitigation and remediation tool.

Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

PubMed

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

A simultaneous analysis method of polycyclic aromatic hydrocarbons, nicotine, cotinine and metals in human hair.

PubMed

Li, Zhenjiang; Wang, Bin; Ge, Shufang; Yan, Lailai; Liu, Yingying; Li, Zhiwen; Ren, Aiguo

2016-12-01

Polycyclic aromatic hydrocarbons (PAHs), nicotine, cotinine, and metals in human hair have been used as important environmental exposure markers. We aimed to develop a simple method to simultaneously analyze these pollutants using a small quantity of hair. The digestion performances of tetramethylammonium hydroxide (TMAH) and sodium hydroxide (NaOH) for human hair were compared. Various solvents or their mixtures including n-hexane (HEX), dichloromethane (DCM) and trichloromethane (TCM), HEX:DCM32 (3/2) and HEX:TCM73 (7/3) were adopted to extract organics. The recoveries of metals were determined under an optimal operation of digestion and extraction. Our results showed that TMAH performed well in dissolving human hair and even better than NaOH. Overall, the recoveries for five solutions were acceptable for PAHs, nicotine in the range of 80%-110%. Except for HEX, other four extraction solutions had acceptable extraction efficiency for cotinine from HEX:TCM73 (88 ± 4.1%) to HEX:DCM32 (100 ± 2.8%). HEX:DCM32 was chosen as the optimal solvent in consideration of its extraction efficiency and lower density than water. The recoveries of 12 typical major or trace metals were mainly in the range of 90%-110% and some of them were close to 100%. In conclusion, the simultaneous analysis of PAHs, nicotine, cotinine, and metals was feasible. Our study provided a simple and low-cost technique for environmental epidemiological studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

A simple and rapid radiochemical choline acetyltransferase (ChAT) assay screening test.

PubMed

Shiba, Kazuhiro; Ogawa, Kazuma; Kinuya, Seigo; Yajima, Kazuyoshi; Mori, Hirofumi

2006-10-15

A simple radiochemical choline acetyltransferase (ChAT) assay screening test was developed by measuring for [(3)H]acetylcholine ([(3)H]ACh) formed from 0.2 mM [(3)H]acetyl-coenzyme A ([(3)H]acetyl-CoA) and 1 mM choline by 0.2 mg of rat brain homogenates containing ChAT into 96-well microplates. A simple and rapid procedure for isolating [(3)H]ACh from the incubation mixture into 96-well microplates was achieved by using a sodium tetraphenylboron (Kalibor) solution (in ethyl acetate, 0.75%, w/v) and a hydrophobic liquid scintillator mixture (1:5, v/v, 0.2 mL) as an extraction solvent. The benefits of this radiochemical method using 96-well microplates are as follows: (1) this method is reliable and reproducible; (2) many samples can be examined at the same time by this method; (3) this method is economical and effective in reducing radioactive waste. The development of a new simple radiochemical ChAT assay screening test is the first stage of development of radiolabeled ChAT mapping agent.

Densitometric HPTLC analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams.

PubMed

Alam, Prawez

2013-08-01

To develop and validate a simple, accurate HPTLC method for the analysis of 8-gingerol and to determine the quantity of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams. The analysis was performed on 10×20 cm aluminium-backed plates coated with 0.2 mm layers of silica gel 60 F254 (E-Merck, Germany) with n-hexane: ethyl acetate 60: 40 (v/v) as mobile phase. Camag TLC Scanner III was used for the UV densitometric scanning at 569. This system was found to give a compact spot of 8-gingerol at retention factor (Rf) value of (0.39±0.04) and linearity was found in the ranges 50-500 ng/spot (r (2)=0.9987). Limit of detection (12.76 ng/spot), limit of quantification (26.32 ng/spot), accuracy (less than 2 %) and recovery (ranging from 98.22-99.20) were found satisfactory. The HPTLC method developed for quantification of 8-gingerol was found to be simple, accurate, reproducible, sensitive and is applicable to the analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams.

Comparison of Different Protein Extraction Methods for Gel-Based Proteomic Analysis of Ganoderma spp.

PubMed

Al-Obaidi, Jameel R; Saidi, Noor Baity; Usuldin, Siti Rokhiyah Ahmad; Hussin, Siti Nahdatul Isnaini Said; Yusoff, Noornabeela Md; Idris, Abu Seman

2016-04-01

Ganoderma species are a group of fungi that have the ability to degrade lignin polymers and cause severe diseases such as stem and root rot and can infect economically important plants and perennial crops such as oil palm, especially in tropical countries such as Malaysia. Unfortunately, very little is known about the complex interplay between oil palm and Ganoderma in the pathogenesis of the diseases. Proteomic technologies are simple yet powerful tools in comparing protein profile and have been widely used to study plant-fungus interaction. A critical step to perform a good proteome research is to establish a method that gives the best quality and a wide coverage of total proteins. Despite the availability of various protein extraction protocols from pathogenic fungi in the literature, no single extraction method was found suitable for all types of pathogenic fungi. To develop an optimized protein extraction protocol for 2-DE gel analysis of Ganoderma spp., three previously reported protein extraction protocols were compared: trichloroacetic acid, sucrose and phenol/ammonium acetate in methanol. The third method was found to give the most reproducible gels and highest protein concentration. Using the later method, a total of 10 protein spots (5 from each species) were successfully identified. Hence, the results from this study propose phenol/ammonium acetate in methanol as the most effective protein extraction method for 2-DE proteomic studies of Ganoderma spp.

The problem of the second wind turbine - a note on a common but flawed wind power estimation method

NASA Astrophysics Data System (ADS)

Gans, F.; Miller, L. M.; Kleidon, A.

2012-06-01

Several recent wind power estimates suggest that this renewable energy resource can meet all of the current and future global energy demand with little impact on the atmosphere. These estimates are calculated using observed wind speeds in combination with specifications of wind turbine size and density to quantify the extractable wind power. However, this approach neglects the effects of momentum extraction by the turbines on the atmospheric flow that would have effects outside the turbine wake. Here we show with a simple momentum balance model of the atmospheric boundary layer that this common methodology to derive wind power potentials requires unrealistically high increases in the generation of kinetic energy by the atmosphere. This increase by an order of magnitude is needed to ensure momentum conservation in the atmospheric boundary layer. In the context of this simple model, we then compare the effect of three different assumptions regarding the boundary conditions at the top of the boundary layer, with prescribed hub height velocity, momentum transport, or kinetic energy transfer into the boundary layer. We then use simulations with an atmospheric general circulation model that explicitly simulate generation of kinetic energy with momentum conservation. These simulations show that the assumption of prescribed momentum import into the atmospheric boundary layer yields the most realistic behavior of the simple model, while the assumption of prescribed hub height velocity can clearly be disregarded. We also show that the assumptions yield similar estimates for extracted wind power when less than 10% of the kinetic energy flux in the boundary layer is extracted by the turbines. We conclude that the common method significantly overestimates wind power potentials by an order of magnitude in the limit of high wind power extraction. Ultimately, environmental constraints set the upper limit on wind power potential at larger scales rather than detailed engineering specifications of wind turbine design and placement.

A simple and fast method based on mixed hemimicelles coated magnetite nanoparticles for simultaneous extraction of acidic and basic pollutants.

PubMed

Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira

2016-01-01

One of the considerable and disputable areas in analytical chemistry is a single-step simultaneous extraction of acidic and basic pollutants. In this research, a simple and fast coextraction of acidic and basic pollutants (with different polarities) with the aid of magnetic dispersive micro-solid phase extraction based on mixed hemimicelles assembly was introduced for the first time. Cetyltrimethylammonium bromide (CTAB)-coated Fe3O4 nanoparticles as an efficient sorbent was successfully applied to adsorb 4-nitrophenol and 4-chlorophenol as two acidic and chlorinated aromatic amines as basic model compounds. Using a central composite design methodology combined with desirability function approach, the optimal experimental conditions were evaluated. The opted conditions were pH = 10; concentration of CTAB = 0.86 mmol L(-1); sorbent amount = 55.5 mg; sorption time = 11.0 min; no salt addition to the sample, type, and volume of the eluent = 120 μL methanol containing 5% acetic acid and 0.01 mol L(-1) HCl; and elution time = 1.0 min. Under the optimum conditions, detection limits and linear dynamic ranges were achieved in the range of 0.05-0.1 and 0.25-500 μg L(-1), respectively. The percent of extraction recoveries and relative standard deviations (n = 5) were in the range of 71.4-98.0 and 4.5-6.5, respectively. The performance of the optimized method was certified by coextraction of other acidic and basic compounds. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of the target analytes in various water samples, and satisfactory results were obtained.

Application of PLE for the determination of essential oil components from Thymus vulgaris L.

PubMed

Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

2008-08-15

Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

PubMed

Ma, Chun-hui; Liu, Ting-ting; Yang, Lei; Zu, Yuan-gang; Chen, Xiaoqiang; Zhang, Lin; Zhang, Ying; Zhao, Chunjian

2011-12-02

Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation. Copyright © 2011 Elsevier B.V. All rights reserved.

Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon followed by high performance liquid chromatography for determination of Sudan dyes in different species.

PubMed

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2018-04-01

In this work, a novel method, namely centrifugeless dispersive liquid-liquid microextraction, is introduced for the efficient extraction of banned Sudan dyes from foodstuff and water samples. In this method, which is based upon the salting-out phenomenon, in order to accelerate the extraction process, the extraction solvent (1-undecanol, 75 μL) is dispersed into the sample solution. Then the mixture is passed through a small column filled with 5 g sodium chloride, used as a separating reagent. In this condition, fine droplets of the extraction solvent are floated on the mixture, and the phase separation is simply achieved. This method is environmentally friendly, simple, and very fast, so that the overall extraction time is only 7 min. Under the optimal experimental conditions, the preconcentration factors in the range of 90-121 were obtained for the analytes. Also good linearities were obtained in the range of 2.5-1200 ng mL -1 (r 2  ≥ 0.993). Copyright © 2017 Elsevier Ltd. All rights reserved.

[Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

PubMed

Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

2014-03-01

Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

[Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

PubMed

Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

2011-02-01

A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

Quantitative analysis of amoxicillin, its major metabolites and ampicillin in eggs by liquid chromatography combined with electrospray ionization tandem mass spectrometry.

PubMed

Sun, Lirui; Jia, Longfei; Xie, Xing; Xie, Kaizhou; Wang, Jianfeng; Liu, Jianyu; Cui, Lulu; Zhang, Genxi; Dai, Guojun; Wang, Jinyu

2016-02-01

In this present study, we developed a simple, rapid and specific method for the quantitative analysis of the contents of amoxicillin (AMO), AMO metabolites and ampicillin (AMP) in eggs. This method uses a simple liquid-liquid extraction with acetonitrile followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The optimized method has been validated according to requirements defined by the European Union and Food and Drug Administration. Extraction recoveries of the target compounds from the egg at 5, 10 and 25 μg/kg were all higher than 80%, with relative standard deviations not exceeding 10.00%. The limits of quantification in eggs were below the maximum residue limits (MRLs). The decision limits (CCα) ranged between 11.1 and 11.5 μg/kg, while detection capabilities (CCβ) from 12.1 to 13.0 μg/kg. These values were very close to the corresponding MRLs. Finally, the new approach was successfully verified for the quantitative determination of these analytes in 40 commercial eggs from local supermarkets. Copyright © 2015 Elsevier Ltd. All rights reserved.

Ionic liquid-based microwave-assisted extraction of flavonoids from Bauhinia championii (Benth.) Benth.

PubMed

Xu, Wei; Chu, Kedan; Li, Huang; Zhang, Yuqin; Zheng, Haiyin; Chen, Ruilan; Chen, Lidian

2012-12-03

An ionic liquids (IL)-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth.) Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE) conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br) solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE) and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min). The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.)Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth.) Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.

PubMed

Golovko, Oksana; Koba, Olga; Kodesova, Radka; Fedorova, Ganna; Kumar, Vimal; Grabic, Roman

2016-07-01

The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram).

Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

2016-01-15

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis

PubMed Central

Zanchetti Meneghini, Leonardo; Rübensam, Gabriel; Claudino Bica, Vinicius; Ceccon, Amanda; Barreto, Fabiano; Flores Ferrão, Marco; Bergold, Ana Maria

2014-01-01

A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences (p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed. PMID:25380457

The Extraction of Terrace in the Loess Plateau Based on radial method

NASA Astrophysics Data System (ADS)

Liu, W.; Li, F.

2016-12-01

The terrace of Loess Plateau, as a typical kind of artificial landform and an important measure of soil and water conservation, its positioning and automatic extraction will simplify the work of land use investigation. The existing methods of terrace extraction mainly include visual interpretation and automatic extraction. The manual method is used in land use investigation, but it is time-consuming and laborious. Researchers put forward some automatic extraction methods. For example, Fourier transform method can recognize terrace and find accurate position from frequency domain image, but it is more affected by the linear objects in the same direction of terrace; Texture analysis method is simple and have a wide range application of image processing. The disadvantage of texture analysis method is unable to recognize terraces' edge; Object-oriented is a new method of image classification, but when introduce it to terrace extracting, fracture polygons will be the most serious problem and it is difficult to explain its geological meaning. In order to positioning the terraces, we use high- resolution remote sensing image to extract and analyze the gray value of the pixels which the radial went through. During the recognition process, we firstly use the DEM data analysis or by manual selecting, to roughly confirm the position of peak points; secondly, take each of the peak points as the center to make radials in all directions; finally, extracting the gray values of the pixels which the radials went through, and analyzing its changing characteristics to confirm whether the terrace exists. For the purpose of getting accurate position of terrace, terraces' discontinuity, extension direction, ridge width, image processing algorithm, remote sensing image illumination and other influence factors were fully considered when designing the algorithms.

Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

PubMed

Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

2016-04-01

A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) < 6% and a recovery of 92-108%. Ultra-high sensitivity, as well as much less sample and reagent consumption and low operating cost, make our method a valuable technique to the speciation analysis of ultra-trace mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of magnetic graphene @hydrophilic polydopamine for the enrichment and analysis of phthalates in environmental water samples.

PubMed

Wang, Xianying; Song, Guoxin; Deng, Chunhui

2015-01-01

Magnetic graphene @hydrophilic polydopamine composites were successfully fabricated via a simple solvothermal reaction and self-polymerization of dopamine. Benefit from the excellent characteristics of strong magnetic responsivity, super-hydrophilicity and abundant π-electron system, the prepared material showed great potential as a magnetic solid phase extraction (MSPE) sorbent. In this work, six kinds of phthalates (PAEs) were selected as the target analytes to evaluate the extraction ability of the adsorbents combined with MSPE-GC-MS. And various extraction parameters were optimized by selecting the pH value of samples, the amount of sorbents, adsorption and desorption time, the type and volume of eluting solution. Meanwhile, the whole extraction process could be finished in 30 min. Under the optimized conditions, validations of the method were evaluated as well. And the results presented excellent linearity with a wide range of 50-20,000 μg/L (R(2)>0.9991). The detection of limits were in the range from 0.05-5 μg/L (S/N=3). Therefore, the novel magnetic graphene@polydopamine composites were successfully used as the sorbents for the enrichment and analysis of PAEs in real water samples. This proposed method provided a simple, efficient and sensitive approach for the determination of aromatic compounds in real environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Facile preparation of magnetic molecularly imprinted polymers for the selective extraction and determination of dexamethasone in skincare cosmetics using HPLC.

PubMed

Du, Wei; Zhang, Bilin; Guo, Pengqi; Chen, Guoning; Chang, Chun; Fu, Qiang

2018-03-15

Dexamethasone-imprinted polymers were fabricated by reversible addition-fragmentation chain transfer polymerization on the surface of magnetic nanoparticles under mild polymerization conditions, which exhibited a narrow polydispersity and high selectivity for dexamethasone extraction. The dexamethasone-imprinted polymers were characterized by scanning electron microscopy, transmission electron microscope, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive spectrometry, and vibrating sample magnetometry. The adsorption performance was evaluated by static adsorption, kinetic adsorption and selectivity tests. The results confirmed the successful construction of an imprinted polymer layer on the surface of the magnetic nanoparticles, which benefits the characteristics of high adsorption capacity, fast mass transfer, specific molecular recognition, and simple magnetic separation. Combined with high-performance liquid chromatography, molecularly imprinted polymers as magnetic extraction sorbents were used for the rapid and selective extraction and determination of dexamethasone in skincare cosmetic samples, with the accuracies of the spiked samples ranging from 93.8 to 97.6%. The relative standard deviations were less than 2.7%. The limit of detection and limit of quantification were 0.05 and 0.20 μg/mL, respectively. The developed method was simple, fast and highly selective and could be a promising method for dexamethasone monitoring in cosmetic products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of spike-sorting algorithms for future hardware implementation.

PubMed

Gibson, Sarah; Judy, Jack W; Markovic, Dejan

2008-01-01

Applications such as brain-machine interfaces require hardware spike sorting in order to (1) obtain single-unit activity and (2) perform data reduction for wireless transmission of data. Such systems must be low-power, low-area, high-accuracy, automatic, and able to operate in real time. Several detection and feature extraction algorithms for spike sorting are described briefly and evaluated in terms of accuracy versus computational complexity. The nonlinear energy operator method is chosen as the optimal spike detection algorithm, being most robust over noise and relatively simple. The discrete derivatives method [1] is chosen as the optimal feature extraction method, maintaining high accuracy across SNRs with a complexity orders of magnitude less than that of traditional methods such as PCA.

Development and validation of an RP-HPLC method for quantitative determination of vanillin and related phenolic compounds in Vanilla planifolia.

PubMed

Sinha, Arun Kumar; Verma, Subash Chandra; Sharma, Upendra Kumar

2007-01-01

A simple and fast method was developed using RP-HPLC for separation and quantitative determination of vanillin and related phenolic compounds in ethanolic extract of pods of Vanilla planifolia. Ten phenolic compounds, namely 4-hydroxybenzyl alcohol, vanillyl alcohol, 3,4-dihydroxybenzaldehyde, 4-hydroxybenzoic acid, vanillic acid, 4-hydroxybenzaldehyde, vanillin, p-coumaric acid, ferulic acid, and piperonal were quantitatively determined using ACN, methanol, and 0.2% acetic acid in water as a mobile phase with a gradient elution mode. The method showed good linearity, high precision, and good recovery of compounds of interest. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

Fingerprint chromatogram analysis of extracts from the leaves of Tripterygium wilfordii Hook. F. by high performance liquid chromatography.

PubMed

Li, Ke; Wang, Shudong

2005-05-01

A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated for the study of fingerprint chromatograms of extracts from the leaves of Tripterygium wilfordii Hook. F. (TWHF) and for controlling the quality of the herb. HPLC separation of the extracts was performed on a Lichrospher RP-18 column and detected by ultraviolet absorbance at 210 nm. The column temperature was maintained at 35 degrees C. A mobile phase composed of acetonitrile:H2O in the ratio of 39:61 (v/v) was found to be most suitable for this separation at a flow rate of 0.8 mL/min with isocratic elution. Under the chromatographic conditions described, the peak profile of the 10 components collected within 35 min made up the fingerprint of the extracts from leaves of TWHF with universal features. The fingerprint chromatograms had a good stability, precision, and reproducibility. The similarity of the extracts from leaves of TWHF collected in summer and winter was studied with triptolide as a reference peak. The method is suitable for differentiation of extracts from the leaves of TWHF, and can be used as a quality control method for this herb.

Deep feature extraction and combination for synthetic aperture radar target classification

NASA Astrophysics Data System (ADS)

Amrani, Moussa; Jiang, Feng

2017-10-01

Feature extraction has always been a difficult problem in the classification performance of synthetic aperture radar automatic target recognition (SAR-ATR). It is very important to select discriminative features to train a classifier, which is a prerequisite. Inspired by the great success of convolutional neural network (CNN), we address the problem of SAR target classification by proposing a feature extraction method, which takes advantage of exploiting the extracted deep features from CNNs on SAR images to introduce more powerful discriminative features and robust representation ability for them. First, the pretrained VGG-S net is fine-tuned on moving and stationary target acquisition and recognition (MSTAR) public release database. Second, after a simple preprocessing is performed, the fine-tuned network is used as a fixed feature extractor to extract deep features from the processed SAR images. Third, the extracted deep features are fused by using a traditional concatenation and a discriminant correlation analysis algorithm. Finally, for target classification, K-nearest neighbors algorithm based on LogDet divergence-based metric learning triplet constraints is adopted as a baseline classifier. Experiments on MSTAR are conducted, and the classification accuracy results demonstrate that the proposed method outperforms the state-of-the-art methods.

Optimization of cloud point extraction and solid phase extraction methods for speciation of arsenic in natural water using multivariate technique.

PubMed

Baig, Jameel A; Kazi, Tasneem G; Shah, Abdul Q; Arain, Mohammad B; Afridi, Hassan I; Kandhro, Ghulam A; Khan, Sumaira

2009-09-28

The simple and rapid pre-concentration techniques viz. cloud point extraction (CPE) and solid phase extraction (SPE) were applied for the determination of As(3+) and total inorganic arsenic (iAs) in surface and ground water samples. The As(3+) was formed complex with ammonium pyrrolidinedithiocarbamate (APDC) and extracted by surfactant-rich phases in the non-ionic surfactant Triton X-114, after centrifugation the surfactant-rich phase was diluted with 0.1 mol L(-1) HNO(3) in methanol. While total iAs in water samples was adsorbed on titanium dioxide (TiO(2)); after centrifugation, the solid phase was prepared to be slurry for determination. The extracted As species were determined by electrothermal atomic absorption spectrometry. The multivariate strategy was applied to estimate the optimum values of experimental factors for the recovery of As(3+) and total iAs by CPE and SPE. The standard addition method was used to validate the optimized methods. The obtained result showed sufficient recoveries for As(3+) and iAs (>98.0%). The concentration factor in both cases was found to be 40.

Determination of rhenium content in molybdenite by ICP-MS after separation of the major matrix by solvent extraction with N-benzoyl-N-phenylhydroxalamine.

PubMed

Li, Jie; Zhong, Li-feng; Tu, Xiang-lin; Liang, Xi-rong; Xu, Ji-feng

2010-05-15

A simple and rapid analytical method for determining the concentration of rhenium in molybdenite for Re-Os dating was developed. The method used isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS) after the removal of major matrix elements (e.g., Mo, Fe, and W) from Re by solvent extraction with N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform solution. The effect on extraction efficiency of parameters such as pH (HCl concentration), BPHA concentration, and extraction time were also assessed. Under the optimal experimental conditions, the validity of the separation method was accessed by measuring (187)Re/(185)Re values for a molybdenite reference material (JDC). The obtained values were in good agreement with previously measured values of the Re standard. The proposed method was applied to replicate Re-Os dating of JDC and seven samples of molybdenite from the Yuanzhuding large Cu-Mo porphyry deposit. The results demonstrate good precision and accuracy for the proposed method. The advantages of the method (i.e., simplicity, efficiency, short analysis time, and low cost) make it suitable for routine analysis.

Rapid and efficient method to extract metagenomic DNA from estuarine sediments.

PubMed

Shamim, Kashif; Sharma, Jaya; Dubey, Santosh Kumar

2017-07-01

Metagenomic DNA from sediments of selective estuaries of Goa, India was extracted using a simple, fast, efficient and environment friendly method. The recovery of pure metagenomic DNA from our method was significantly high as compared to other well-known methods since the concentration of recovered metagenomic DNA ranged from 1185.1 to 4579.7 µg/g of sediment. The purity of metagenomic DNA was also considerably high as the ratio of absorbance at 260 and 280 nm ranged from 1.88 to 1.94. Therefore, the recovered metagenomic DNA was directly used to perform various molecular biology experiments viz. restriction digestion, PCR amplification, cloning and metagenomic library construction. This clearly proved that our protocol for metagenomic DNA extraction using silica gel efficiently removed the contaminants and prevented shearing of the metagenomic DNA. Thus, this modified method can be used to recover pure metagenomic DNA from various estuarine sediments in a rapid, efficient and eco-friendly manner.

[Study on molecular recognition technology in active constituents extracted and isolated from Aconitum pendulum].

PubMed

Ma, Xue-Qin; Li, Guo-Shan; Fu, Xue-Yan; Ma, Jing-Zu

2011-03-01

To investigate CD molecular recognition technology applied in active constituents extracted and isolated from traditional Chinese medicine--Aconitum pendulum. The inclusion constant and form probability of the inclusion complex of Aconitum pendulum with p-CD was calculated by UV spectra method. The active constituents of Aconitum pendulum were extracted and isolated by molecular recognition technology. The inclusion complex was identified by UV. The chemical constituents of Aconitum pendulum and inclusion complex was determined by HPLC. The analgesic effects of inclusion complex was investigated by experiment of intraperitoneal injection of acetic acid in rats. The inclusion complex was identified and confirmed by UV spectra method, the chemical components of inclusion complex were simple, and the content of active constituents increased significantly, the analgesic effects of inclusion complex was well. The molecular recognition technology can be used for extracting and isolating active constituents of Aconitum pendulum, and the effects are obvious.

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

PubMed

Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

2014-06-05

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.

Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

PubMed

Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

2013-01-01

A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

USGS Publications Warehouse

Datta, S.; Do, L.V.; Young, T.M.

2004-01-01

A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

Respiratory-phase domain analysis of heart rate variability can accurately estimate cardiac vagal activity during a mental arithmetic task.

PubMed

Kotani, Kiyoshi; Takamasu, Kiyoshi; Tachibana, Makoto

2007-01-01

The objectives of this paper were to present a method to extract the amplitude of RSA in the respiratory-phase domain, to compare that with subjective or objective indices of the MWL (mental workload), and to compare that with a conventional frequency analysis in terms of its accuracy during a mental arithmetic task. HRV (heart rate variability), ILV (instantaneous lung volume), and motion of the throat were measured under a mental arithmetic experiment and subjective and objective indices were also obtained. The amplitude of RSA was extracted in the respiratory-phase domain, and its correlation with the load level was compared with the results of the frequency domain analysis, which is the standard analysis of the HRV. The subjective and objective indices decreased as the load level increased, showing that the experimental protocol was appropriate. Then, the amplitude of RSA in the respiratory-phase domain also decreased with the increase in the load level. The results of the correlation analysis showed that the respiratory-phase domain analysis has higher negative correlations, -0.84 and -0.82, with the load level as determined by simple correlation and rank correlation, respectively, than does frequency analysis, for which the correlations were found to be -0.54 and -0.63, respectively. In addition, it was demonstrated that the proposed method could be applied to the short-term extraction of RSA amplitude. We proposed a simple and effective method to extract the amplitude of the respiratory sinus arrhythmia (RSA) in the respiratory-phase domain and the results show that this method can estimate cardiac vagal activity more accurately than frequency analysis.

Built-up Areas Extraction in High Resolution SAR Imagery based on the method of Multiple Feature Weighted Fusion

NASA Astrophysics Data System (ADS)

Liu, X.; Zhang, J. X.; Zhao, Z.; Ma, A. D.

2015-06-01

Synthetic aperture radar in the application of remote sensing technology is becoming more and more widely because of its all-time and all-weather operation, feature extraction research in high resolution SAR image has become a hot topic of concern. In particular, with the continuous improvement of airborne SAR image resolution, image texture information become more abundant. It's of great significance to classification and extraction. In this paper, a novel method for built-up areas extraction using both statistical and structural features is proposed according to the built-up texture features. First of all, statistical texture features and structural features are respectively extracted by classical method of gray level co-occurrence matrix and method of variogram function, and the direction information is considered in this process. Next, feature weights are calculated innovatively according to the Bhattacharyya distance. Then, all features are weighted fusion. At last, the fused image is classified with K-means classification method and the built-up areas are extracted after post classification process. The proposed method has been tested by domestic airborne P band polarization SAR images, at the same time, two groups of experiments based on the method of statistical texture and the method of structural texture were carried out respectively. On the basis of qualitative analysis, quantitative analysis based on the built-up area selected artificially is enforced, in the relatively simple experimentation area, detection rate is more than 90%, in the relatively complex experimentation area, detection rate is also higher than the other two methods. In the study-area, the results show that this method can effectively and accurately extract built-up areas in high resolution airborne SAR imagery.

Rapid isothermal detection of Phytophthora species on plant samples using recombinase polymerase amplification

USDA-ARS?s Scientific Manuscript database

Recently several isothermal amplification techniques have been developed that are extremely tolerant towards inhibitors present in many plant extracts. Recombinase polymerase amplification (RPA) assays for the genus Phytophthora have been developed which provide a simple and rapid method to macerate...

A cockspur for the DSS cells: Erythrina crista-galli sensitizers

NASA Astrophysics Data System (ADS)

Enciso, Paula; Decoppet, Jean-David; Grätzel, Michael; Wörner, Michael; Cabrerizo, Franco M.; Cerdá, María Fernanda

2017-04-01

Dye sensitized solar cells were assembled employing a mixture of anthocyanins extracted from red ceibo's flowers. At the literature different extraction procedures are reported to extract anthocyanins from natural products and sensitize the cells. In order to compare them, different methods were followed to set the cells under the same conditions. Assembled cells showed very interesting conversion efficiency values, reaching a 0.73% value for extracts purified using C18 column, in open cells under illumination using a solar light simulator, 1 sun, 1.5 AM. Data reported herein prove that anthocyanins obtained from ceibo's flower, after simple further purification, might represent an excellent, cheap and clean alternative for the development of DSS cells.

Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

2015-09-30

A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

Uncertainties in forces extracted from non-contact atomic force microscopy measurements by fitting of long-range background forces.

PubMed

Sweetman, Adam; Stannard, Andrew

2014-01-01

In principle, non-contact atomic force microscopy (NC-AFM) now readily allows for the measurement of forces with sub-nanonewton precision on the atomic scale. In practice, however, the extraction of the often desired 'short-range' force from the experimental observable (frequency shift) is often far from trivial. In most cases there is a significant contribution to the total tip-sample force due to non-site-specific van der Waals and electrostatic forces. Typically, the contribution from these forces must be removed before the results of the experiment can be successfully interpreted, often by comparison to density functional theory calculations. In this paper we compare the 'on-minus-off' method for extracting site-specific forces to a commonly used extrapolation method modelling the long-range forces using a simple power law. By examining the behaviour of the fitting method in the case of two radically different interaction potentials we show that significant uncertainties in the final extracted forces may result from use of the extrapolation method.

Sensitive quantitation of polyamines in plant foods by ultrasound-assisted benzoylation and dispersive liquid-liquid microextraction with the aid of experimental designs.

PubMed

Pinto, Edgar; Melo, Armindo; Ferreira, Isabel M P L V O

2014-05-14

A new method involving ultrasound-assisted benzoylation and dispersive liquid-liquid microextraction was optimized with the aid of chemometrics for the extraction, cleanup, and determination of polyamines in plant foods. Putrescine, cadaverine, spermidine, and spermine were derivatized with 3,5-dinitrobenzoyl chloride and extracted by dispersive liquid-liquid microextraction using acetonitrile and carbon tetrachloride as dispersive and extraction solvents, respectively. Two-level full factorial design and central composite design were applied to select the most appropriate derivatization and extraction conditions. The developed method was linear in the 0.5-10.0 mg/L range, with a R(2) ≥ 0.9989. Intra- and interday precisions ranged from 0.8 to 6.9% and from 3.0 to 10.3%, respectively, and the limit of detection ranged between 0.018 and 0.042 μg/g of fresh weight. This method was applied to the analyses of six different types of plant foods, presenting recoveries between 81.7 and 114.2%. The method is inexpensive, versatile, simple, and sensitive.

A rapid and simple determination of caffeine in teas, coffees and eight beverages.

PubMed

Sereshti, Hassan; Samadi, Soheila

2014-09-01

Caffeine was extracted and preconcentrated by the simple, fast and green method of dispersive liquid-liquid microextraction (DLLME) and analysed by gas chromatography-nitrogen phosphorus detection (GC-NPD). The influence of main parameters affecting the extraction efficiency investigated and optimised. Under the optimal conditions, the method was successfully applied to determination of caffeine in different real samples including five types of tea (green, black, white, oolong teas and tea bag), two kinds of coffee (Nescafe coffee and coffee), and eight beverages (regular Coca Cola, Coca Cola zero, regular Pepsi, Pepsi max, Sprite, 7up, Red Bull and Hype).The limit of detection (LOD) and limit of quantification (LOQ) were 0.02 and 0.05 μg mL(-1), respectively. Linear dynamic range (LDR) was 0.05-500 μg mL(-1) and determination coefficient (R(2)) was 0.9990. The relative standard deviation (RSD) was 3.2% (n=5, C=1 μg mL(-1)). Copyright © 2014 Elsevier Ltd. All rights reserved.

Simple procedures for enrichment of chlorinated aromatic pollutants from fat, water and milk for subsequent analysis by high-resolution methods

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

Egestad, B.; Curstedt, T.; Sjoevall, J.

1982-01-01

Procedures for enrichment of non-volatile chlorinated aromatic pollutants from fat, water and milk are described. /sup 14/C-DDT was used as a model compound in recovery experiments. A several thousand-fold enrichment of DDT added to butter was achieved by two consecutive straight-phase chromatographies on Lipidex 5000. Trace amounts of DDT in liter volumes of water could be quantitatively extracted by rapid filtration through 2 ml beds of Lipidex 1000. A batch extraction procedure permitted enrichment of DDT from milk after addition of n-pentylamine, methanol and water. DDT could then be eluted from the gel with retention of more than 90% ofmore » the lipids. A reversed-phase system with Lipidex 5000 could be used for separation of TCDD from DDT and PCBs. The liquid-gel chromatographic procedures are simple and suitable for clean-up of samples prior to application of high-resolution methods. 5 tables.« less

Evaluation of thin-layer chromatography methods for quality control of commercial products containing Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis.

PubMed

Ramírez-Durón, Rosalba; Ceniceros-Almaguer, Lucía; Salazar-Aranda, Ricardo; Salazar-Cavazos, Ma de la Luz; Waksman de Torres, Noemi

2007-01-01

In Mexico, plant-derived products with health claims are sold as herbal dietary supplements, and there are no rules for their legal quality control. Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis are some of the major commercial products obtained from plants used in this region. In this paper, we describe the effectiveness of thin-layer chromatography methods to provide for the quality control of several commercial products containing these plants. Standardized extracts were used. Of the 49 commercial products analyzed, only 32.65% matched the chromatographic characteristic of standardized extracts. A significant number of commercial products did not match their label, indicating a problem resulting from the lack of regulation for these products. The proposed methods are simple, sensitive, and specific and can be used for routine quality control of raw herbals and formulations of the tested plants. The results obtained show the need to develop simple and reliable analytical methods that can be performed in any laboratory for the purpose of quality control of dietary supplements or commercial herbal products sold in Mexico.

Eco-friendly ionic liquid based ultrasonic assisted selective extraction coupled with a simple liquid chromatography for the reliable determination of acrylamide in food samples.

PubMed

Albishri, Hassan M; El-Hady, Deia Abd

2014-01-01

Acrylamide in food has drawn worldwide attention since 2002 due to its neurotoxic and carcinogenic effects. These influences brought out the dual polar and non-polar characters of acrylamide as they enabled it to dissolve in aqueous blood medium or penetrate the non-polar plasma membrane. In the current work, a simple HPLC/UV system was used to reveal that the penetration of acrylamide in non-polar phase was stronger than its dissolution in polar phase. The presence of phosphate salts in the polar phase reduced the acrylamide interaction with the non-polar phase. Furthermore, an eco-friendly and costless coupling of the HPLC/UV with ionic liquid based ultrasonic assisted extraction (ILUAE) was developed to determine the acrylamide content in food samples. ILUAE was proposed for the efficient extraction of acrylamide from bread and potato chips samples. The extracts were obtained by soaking of potato chips and bread samples in 1.5 mol L(-1) 1-butyl-3-methylimmidazolium bromide (BMIMBr) for 30.0 and 60.0 min, respectively and subsequent chromatographic separation within 12.0 min using Luna C18 column and 100% water mobile phase with 0.5 mL min(-1) under 25 °C column temperature at 250 nm. The extraction and analysis of acrylamide could be achieved within 2h. The mean extraction efficiency of acrylamide showed adequate repeatability with relative standard deviation (RSD) of 4.5%. The limit of detection and limit of quantitation were 25.0 and 80.0 ng mL(-1), respectively. The accuracy of the proposed method was tested by recovery in seven food samples giving values ranged between 90.6% and 109.8%. Therefore, the methodology was successfully validated by official guidelines, indicating its reliability to be applied to analysis of real samples, proven to be useful for its intended purpose. Moreover, it served as a simple, eco-friendly and costless alternative method over hitherto reported ones. © 2013 Elsevier B.V. All rights reserved.

Assessment of simple colorimetric procedures to determine smoking status of diabetic subjects.

PubMed

Smith, R F; Mather, H M; Ellard, G A

1998-02-01

The performance of a simple colorimetric assay for urinary nicotine metabolites to assess smoking status in diabetic subjects (n = 251) was investigated. Several variations of the colorimetric assay and a qualitative extraction procedure were evaluated in comparison with a cotinine immunoassay as the "gold standard." Among these, the best overall performance was achieved with the qualitative test (sensitivity 95%; specificity 100%). The quantitative measurement of total nicotine metabolites performed less well (sensitivity 92%; specificity 97%) but could be improved by incorporating a blank extraction (sensitivity 98%; specificity 98%). Allowance for diuresis appeared to offer no advantage over the other methods. These results support previous findings regarding the use of these colorimetric procedures in nondiabetic subjects and, contrary to other recent observations, their performance was not impaired in diabetic patients.

Fluorescent carbon nanodots facilely extracted from Coca Cola for temperature sensing

NASA Astrophysics Data System (ADS)

Li, Feiming; Chen, Qiaoling; Cai, Zhixiong; Lin, Fangyuan; Xu, Wei; Wang, Yiru; Chen, Xi

2017-12-01

A novel method for the fabrication of carbon nanodots (CDs) is introduced: extracting CDs from the well-known soft drink Coca Cola via dialysis. The obtained CDs are of good monodispersity with a narrow size distribution (average diameter of 3.0 nm), good biocompatibility, high solubility (about 180 mg ml-1) and stable fluorescence even at a high salt concentration. Furthermore, they are sensitive to the temperature change with a linear relationship between the fluorescence intensity and temperature from 5 °C-95 °C. The CDs have been applied in high stable temperature sensing. This protocol is quite simple, green, cost-effective and technologically simple, which might be used for a range of applications including sensing, catalysts, drug and gene delivery, and so on.

Fluorescent carbon nanodots facilely extracted from Coca Cola for temperature sensing.

PubMed

Li, Feiming; Chen, Qiaoling; Cai, Zhixiong; Lin, Fangyuan; Xu, Wei; Wang, Yiru; Chen, Xi

2017-10-16

A novel method for the fabrication of carbon nanodots (CDs) is introduced: extracting CDs from the well-known soft drink Coca Cola via dialysis. The obtained CDs are of good monodispersity with a narrow size distribution (average diameter of 3.0 nm), good biocompatibility, high solubility (about 180 mg ml -1 ) and stable fluorescence even at a high salt concentration. Furthermore, they are sensitive to the temperature change with a linear relationship between the fluorescence intensity and temperature from 5 °C-95 °C. The CDs have been applied in high stable temperature sensing. This protocol is quite simple, green, cost-effective and technologically simple, which might be used for a range of applications including sensing, catalysts, drug and gene delivery, and so on.

Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry

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

Wunschel, David S.; Valenzuela, Blandina R.; Kaiser, Brooke L. Deatherage

A variety of toxins are produced by marine and freshwater microorganisms that present a threat to human health. These toxins have diverse chemical properties and specifically, a range of hydrophobicity. Methods for extraction and identification of these toxins are often geared toward specific classes of toxin depending on the sample type. There is a need for a general method of toxin extraction and identification for screening samples where the likely toxin content is not known a priori. Here, we have applied a general method for metabolite extraction to toxin containing samples. This method was coupled with a simple dual liquidmore » chromatography approach for separating a broad range of toxins. This liquid chromatography approach was coupled to triple quadrupole and quadrupole time-of-flight MS/MS platforms. The method was testing on a fish matrix for recovery of palytoxin as well as marine corals for detection of natural mixtures of palytoxin analogues. The recovery of palytoxin was found to produce a linear response (R 2 of 0.95) when spiked into the fish matrix with a limit of quantitation of 2.5 ng/μL and recovery efficiency of 73% +/- 9%. The screening of corals revealed varying amount of palytoxin, and in one case, different palytoxin structural analogues. This demonstration illustrates the potential utility of this method for toxin extraction and detection.« less

Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry

DOE PAGES

Wunschel, David S.; Valenzuela, Blandina R.; Kaiser, Brooke L. Deatherage; ...

2018-05-09

A variety of toxins are produced by marine and freshwater microorganisms that present a threat to human health. These toxins have diverse chemical properties and specifically, a range of hydrophobicity. Methods for extraction and identification of these toxins are often geared toward specific classes of toxin depending on the sample type. There is a need for a general method of toxin extraction and identification for screening samples where the likely toxin content is not known a priori. Here, we have applied a general method for metabolite extraction to toxin containing samples. This method was coupled with a simple dual liquidmore » chromatography approach for separating a broad range of toxins. This liquid chromatography approach was coupled to triple quadrupole and quadrupole time-of-flight MS/MS platforms. The method was testing on a fish matrix for recovery of palytoxin as well as marine corals for detection of natural mixtures of palytoxin analogues. The recovery of palytoxin was found to produce a linear response (R 2 of 0.95) when spiked into the fish matrix with a limit of quantitation of 2.5 ng/μL and recovery efficiency of 73% +/- 9%. The screening of corals revealed varying amount of palytoxin, and in one case, different palytoxin structural analogues. This demonstration illustrates the potential utility of this method for toxin extraction and detection.« less

Evaluation of extraction methods for ochratoxin A detection in cocoa beans employing HPLC.

PubMed

Mishra, Rupesh K; Catanante, Gaëlle; Hayat, Akhtar; Marty, Jean-Louis

2016-01-01

Cocoa is an important ingredient for the chocolate industry and for many food products. However, it is prone to contamination by ochratoxin A (OTA), which is highly toxic and potentially carcinogenic to humans. In this work, four different extraction methods were tested and compared based on their recoveries. The best protocol was established which involves an organic solvent-free extraction method for the detection of OTA in cocoa beans using 1% sodium hydrogen carbonate (NaHCO3) in water within 30 min. The extraction method is rapid (as compared with existing methods), simple, reliable and practical to perform without complex experimental set-ups. The cocoa samples were freshly extracted and cleaned-up using immunoaffinity column (IAC) for HPLC analysis using a fluorescence detector. Under the optimised condition, the limit of detection (LOD) and limit of quantification (LOQ) for OTA were 0.62 and 1.25 ng ml(-1) respectively in standard solutions. The method could successfully quantify OTA in naturally contaminated samples. Moreover, good recoveries of OTA were obtained up to 86.5% in artificially spiked cocoa samples, with a maximum relative standard deviation (RSD) of 2.7%. The proposed extraction method could determine OTA at the level 1.5 µg kg(-)(1), which surpassed the standards set by the European Union for cocoa (2 µg kg(-1)). In addition, an efficiency comparison of IAC and molecular imprinted polymer (MIP) column was also performed and evaluated.

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of Gluten Extraction Protocols Assessed by LC-MS/MS Analysis.

PubMed

Fallahbaghery, Azadeh; Zou, Wei; Byrne, Keren; Howitt, Crispin A; Colgrave, Michelle L

2017-04-05

The efficiency of gluten extraction is of critical importance to the results derived from any analytical method for gluten detection and quantitation, whether it employs reagent-based technology (antibodies) or analytical instrumentation (mass spectrometry). If the target proteins are not efficiently extracted, the end result will be an under-estimation in the gluten content posing a health risk to people affected by conditions such as celiac disease (CD) and nonceliac gluten sensitivity (NCGS). Five different extraction protocols were investigated using LC-MRM-MS for their ability to efficiently and reproducibly extract gluten. The rapid and simple "IPA/DTT" protocol and related "two-step" protocol were enriched for gluten proteins, 55/86% (trypsin/chymotrypsin) and 41/68% of all protein identifications, respectively, with both methods showing high reproducibility (CV < 15%). When using multistep protocols, it was critical to examine all fractions, as coextraction of proteins occurred across fractions, with significant levels of proteins existing in unexpected fractions and not all proteins within a particular gluten class behaving the same.

Extraction of Total Nucleic Acids From Ticks for the Detection of Bacterial and Viral Pathogens

PubMed Central

Crowder, Chris D.; Rounds, Megan A.; Phillipson, Curtis A.; Picuri, John M.; Matthews, Heather E.; Halverson, Justina; Schutzer, Steven E.; Ecker, David J.; Eshoo, Mark W.

2010-01-01

Ticks harbor numerous bacterial, protozoal, and viral pathogens that can cause serious infections in humans and domestic animals. Active surveillance of the tick vector can provide insight into the frequency and distribution of important pathogens in the environment. Nucleic-acid based detection of tick-borne bacterial, protozoan, and viral pathogens requires the extraction of both DNA and RNA (total nucleic acids) from ticks. Traditional methods for nucleic acid extraction are limited to extraction of either DNA or the RNA from a sample. Here we present a simple bead-beating based protocol for extraction of DNA and RNA from a single tick and show detection of Borrelia burgdorferi and Powassan virus from individual, infected Ixodes scapularis ticks. We determined expected yields for total nucleic acids by this protocol for a variety of adult tick species. The method is applicable to a variety of arthropod vectors, including fleas and mosquitoes, and was partially automated on a liquid handling robot. PMID:20180313

A Simple Method for Isolation of Caffeine from Black Tea Leaves: Use of a Dichloromethane-Alkaline Water Mixture as an Extractant

NASA Astrophysics Data System (ADS)

Onami, Tetsuo; Kanazawa, Hitoshi

1996-06-01

A simple procedure for the isolation of caffeine from tea leaves has been established without using hot or boiling water. A mixture of tea leaves, dichloromethane, and 0.2 M NaOH was shaken for 7 min, and the organic layer was separated. After evaporation of the organic solvent, residual crystals were purified by recrystallization to give 20-30 mg (student yield) of pure caffeine from one tea bag (2 g).

[Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

PubMed

Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

2005-10-01

A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS.

A simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry.

PubMed

Martins, Magda Targa; Melo, Jéssica; Barreto, Fabiano; Hoff, Rodrigo Barcellos; Jank, Louise; Bittencourt, Michele Soares; Arsand, Juliana Bazzan; Schapoval, Elfrides Eva Scherman

2014-11-01

In routine laboratory work, screening methods for multiclass analysis can process a large number of samples in a short time. The main challenge is to develop a methodology to detect as many different classes of residues as possible, combined with speed and low cost. An efficient technique for the analysis of multiclass antibacterial residues (fluoroquinolones, tetracyclines, sulfonamides and trimethoprim) was developed based on simple, environment-friendly extraction for bovine milk, cattle and poultry liver. Acidified ethanol was used as an extracting solvent for milk samples. Liver samples were treated using EDTA-washed sand for cell disruption, methanol:water and acidified acetonitrile as extracting solvent. A total of 24 antibacterial residues were detected and confirmed using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), at levels between 10, 25 and 50% of the maximum residue limit (MRL). For liver samples a metabolite (sulfaquinoxaline-OH) was also monitored. A validation procedure was conducted for screening purposes in accordance with European Union requirements (2002/657/EC). The detection capability (CCβ) false compliant rate was less than 5% at the lowest level for each residue. Specificity and ruggedness were also discussed. Incurred and routine samples were analyzed and the method was successfully applied. The results proved that this method can be an important tool in routine analysis, since it is very fast and reliable. Copyright © 2014. Published by Elsevier B.V.

Magnetic solid-phase extraction of heterocyclic pesticides in environmental water samples using metal-organic frameworks coupled to high performance liquid chromatography determination.

PubMed

Ma, Jiping; Wu, Gege; Li, Shuang; Tan, Weiqiang; Wang, Xiaoyan; Li, Jinhua; Chen, Lingxin

2018-06-08

A simple method of magnetic solid-phase extraction (MSPE) coupled to high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of four kinds of heterocyclic pesticides (carbendazim, triadimefon, chlorfenapyr and fenpyroximate) in environmental water samples. Magnetic metal-organic frameworks (MOFs) of type MOF-5 were prepared and used as adsorbents of MSPE. Several main parameters influencing MSPE efficiency were investigated, including amount of magnetic MOF-5, sample solution pH, extraction time, salt concentration, type and volume of desorption solvents and desorption time. Under optimal conditions, the MSPE-HPLC method presented fast simple separation and analysis, and excellent linearity in the range of 0.3-500.0 μg/L for carbendazim and triadimefon, and 0.1-500.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients (r) higher than 0.9992. High sensitivity with limits of detection and quantification ranging from 0.04-0.11 μg/L and 0.13-0.35 μg/L, respectively, were achieved, as well as good precision with relative standard deviations of 2.98-7.11% (intra-day) and 3.31-7.12% (inter-day). Furthermore, the method was successfully applied to reservoir and Yellow River water samples, and satisfactory recoveries at three spiked concentration levels were between 80.20% and 108.33%.The magnetic MOF-5 composites based MSPE followed by HPLC proved promising for convenient and efficient determination of heterocyclic pesticides in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Plant genotyping using fluorescently tagged inter-simple sequence repeats (ISSRs): basic principles and methodology.

PubMed

Prince, Linda M

2015-01-01

Inter-simple sequence repeat PCR (ISSR-PCR) is a fast, inexpensive genotyping technique based on length variation in the regions between microsatellites. The method requires no species-specific prior knowledge of microsatellite location or composition. Very small amounts of DNA are required, making this method ideal for organisms of conservation concern, or where the quantity of DNA is extremely limited due to organism size. ISSR-PCR can be highly reproducible but requires careful attention to detail. Optimization of DNA extraction, fragment amplification, and normalization of fragment peak heights during fluorescent detection are critical steps to minimizing the downstream time spent verifying and scoring the data.

Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

PubMed

Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

2013-07-26

A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

[Developments in preparation and experimental method of solid phase microextraction fibers].

PubMed

Yi, Xu; Fu, Yujie

2004-09-01

Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

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.

Uncovering the spatial structure of mobility networks

NASA Astrophysics Data System (ADS)

Louail, Thomas; Lenormand, Maxime; Picornell, Miguel; García Cantú, Oliva; Herranz, Ricardo; Frias-Martinez, Enrique; Ramasco, José J.; Barthelemy, Marc

2015-01-01

The extraction of a clear and simple footprint of the structure of large, weighted and directed networks is a general problem that has relevance for many applications. An important example is seen in origin-destination matrices, which contain the complete information on commuting flows, but are difficult to analyze and compare. We propose here a versatile method, which extracts a coarse-grained signature of mobility networks, under the form of a 2 × 2 matrix that separates the flows into four categories. We apply this method to origin-destination matrices extracted from mobile phone data recorded in 31 Spanish cities. We show that these cities essentially differ by their proportion of two types of flows: integrated (between residential and employment hotspots) and random flows, whose importance increases with city size. Finally, the method allows the determination of categories of networks, and in the mobility case, the classification of cities according to their commuting structure.

Extracting Characteristics of the Study Subjects from Full-Text Articles

PubMed Central

Demner-Fushman, Dina; Mork, James G

2015-01-01

Characteristics of the subjects of biomedical research are important in determining if a publication describing the research is relevant to a search. To facilitate finding relevant publications, MEDLINE citations provide Medical Subject Headings that describe the subjects’ characteristics, such as their species, gender, and age. We seek to improve the recommendation of these headings by the Medical Text Indexer (MTI) that supports manual indexing of MEDLINE. To that end, we explore the potential of the full text of the publications. Using simple recall-oriented rule-based methods we determined that adding sentences extracted from the methods sections and captions to the abstracts prior to MTI processing significantly improved recall and F1 score with only a slight drop in precision. Improvements were also achieved in directly assigning several headings extracted from the full text. These results indicate the need for further development of automated methods capable of leveraging the full text for indexing. PMID:26958181

Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.

PubMed

Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila

2014-09-01

A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integration of phase separation with ultrasound-assisted salt-induced liquid-liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography.

PubMed

Wang, Huili; Gao, Ming; Wang, Mei; Zhang, Rongbo; Wang, Wenwei; Dahlgren, Randy A; Wang, Xuedong

2015-03-15

Herein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945μL acetone extraction solvent, pH 2.1, 4.1min stir time, 5.9g Na2SO4, and 4.0min centrifugation. Under optimized conditions, the limits of detection (at S/N=3) were 0.12-0.66μgL(-1), the linear range was 0.5-500μgL(-1) and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids. Copyright © 2015 Elsevier B.V. All rights reserved.

Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

PubMed

Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

2016-06-01

Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

ASE extraction method for simultaneous carbon and nitrogen stable isotope analysis in soft tissues of aquatic organisms.

PubMed

Bodin, Nathalie; Budzinski, Hélène; Le Ménach, Karyn; Tapie, Nathalie

2009-06-08

Since lipids are depleted in 13C relative to proteins and carbohydrates, variations in lipid composition among species and within individuals significantly influence delta13C and may result in misleading ecological interpretations. Whereas lipid extraction before IRMS analysis constitutes a way of stable isotope result lipid-normalisation, such a procedure was given up because of the un-controlled effects of the methods used (i.e., "Bligh & Dyer", Soxhlet, etc.) on delta15N. The aim of this work was to develop a simple, rapid and efficient lipid extraction method allowing for simultaneous C and N stable isotope analysis in the biological soft tissues of aquatic organisms. The goal was to be free from the lipid influence on delta13C values without interfering with delta15N values. For that purpose, the modern automated pressurized liquid extraction technique ASE (accelerated solvent extraction) was selected. Eel muscles representative of a broad range of fat contents were extracted via ASE by using different semi-polar solvents (100% dichloromethane and 80% n-hexane/20% acetone) and by operating at different temperature (ambient temperature and 100 degrees C) and pressure (750 and 1900 psi) conditions. The results were discussed in terms of lipid extraction efficiency as well as delta13C and delta15N variability.

Direct extraction of genomic DNA from maize with aqueous ionic liquid buffer systems for applications in genetically modified organisms analysis.

PubMed

Gonzalez García, Eric; Ressmann, Anna K; Gaertner, Peter; Zirbs, Ronald; Mach, Robert L; Krska, Rudolf; Bica, Katharina; Brunner, Kurt

2014-12-01

To date, the extraction of genomic DNA is considered a bottleneck in the process of genetically modified organisms (GMOs) detection. Conventional DNA isolation methods are associated with long extraction times and multiple pipetting and centrifugation steps, which makes the entire procedure not only tedious and complicated but also prone to sample cross-contamination. In recent times, ionic liquids have emerged as innovative solvents for biomass processing, due to their outstanding properties for dissolution of biomass and biopolymers. In this study, a novel, easily applicable, and time-efficient method for the direct extraction of genomic DNA from biomass based on aqueous-ionic liquid solutions was developed. The straightforward protocol relies on extraction of maize in a 10 % solution of ionic liquids in aqueous phosphate buffer for 5 min at room temperature, followed by a denaturation step at 95 °C for 10 min and a simple filtration to remove residual biopolymers. A set of 22 ionic liquids was tested in a buffer system and 1-ethyl-3-methylimidazolium dimethylphosphate, as well as the environmentally benign choline formate, were identified as ideal candidates. With this strategy, the quality of the genomic DNA extracted was significantly improved and the extraction protocol was notably simplified compared with a well-established method.

Magnetic Solid Phase Extraction Based on Oleic Acid Coated Fe3O4 for the Determination of Benzo[α]pyrene in Cigarette Smoke Coupled with High-Performance Liquid Chromatography.

PubMed

Feng, Shouai; Wei, Kang; Tian, Zhaofu; Li, Xiaolan; Meng, Dongling; Liao, Wenlong; Miao, Mingming; Yang, Yaling

2016-07-29

In this work, a simple and effective method based on magnetic solid-phase extraction combined with high-performance liquid chromatography was developed for the determination of benzo[α]pyrene (BaP) in cigarette smoke. Oleic acid coated Fe 3 O 4 (Fe 3 O 4 -OA) was synthesized and directly used as an efficient sorbent for the first time in magnetic solid-phase extraction (MSPE) procedure for the clean-up of BaP in cigarette smoke extracts. The synthesized Fe 3 O 4 -OA was characterized by transmission electron microscopy, X-ray diffraction and Fourier transformed infrared spectroscopy. The extraction via Fe 3 O 4 -OA was dispersed in the extracts of cigarette smoke followed by the magnetic isolation, acetonitrile-tetrahydrofuran (ACN-THF; v/v = 9:1) was used for desorption of the analyte. The effects of important parameters such as the amount of adsorbent, solution pH, the content of acetonitrile, temperature and sorption time were investigated. The method showed good linearity for the determination of BaP in the concentration range of 0.5-50 ng mL -1 with a regression coefficient (R 2 ) of 0.9987. The limit of detection and limit of quantification for BaP were obtained to be 0.12 and 0.41 ng mL -1 , respectively. The mean recoveries were in the range from 81.0% to 97.6% at low, medium, high spiked levels, and the relative standard deviations were in the range of 2.7-6.8%. Combined with high-performance liquid chromatography and fluorescence detection, a simple and effective method was developed for the analysis of BaP in cigarette smoke. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A simple and efficient ultrasonic-assisted extraction procedure combined with UV-Vis spectrophotometry for the pre-concentration and determination of folic acid (vitamin B9) in various sample matrices.

PubMed

Gürkan, Ramazan; Altunay, Nail

2016-07-01

A simple and efficient ultrasonic-assisted extraction (UAE) procedure has been proposed for the pre-concentration of (2S)-2-[(4-{[(2-amino-4-hydroxypteridin-yl)methyl]amino}phenyl)formamido]pentanedioic acid (folic acid) in vegetables, pharmaceuticals and foods prior to determination at 540 nm using UV-Vis spectrophotometry. The method is based on hydrophobic ternary complex formation of folic acid with silver ions in the presence of cetyltrimethylammonium bromide (CTAB) as a sensitivity enhancer counter ion at pH 7.0, and then extraction into a micellar phase of polyethylene glycol monoalkyl ether (Genapol X-080). The impacts on the extraction efficiency and complex formation of analytical parameters such as sample pH, concentration of silver, concentration of surfactants and extraction time, ultrasonic time and sample volume, were investigated and optimised in detail. The matrix effect on the pre-concentration and determination of folic acid was investigated, and it was observed that the proposed method was highly selective against possible matrix co-extractives. Under optimised conditions, a good linear relationship between the analytical signal and folic acid concentration was obtained in the range of 0.6-180 μg l(-1) with a detection limit of 0.19 μg l(-1) and quantification limit of 0.63 μg l(-1). The applicability was evaluated using samples fortified at different concentration levels, and recoveries higher than 94.1% were obtained. The precision as the percent relative standard deviation (RSD%) was in range of 2.5-3.8% (10 and 40 μg l(-1), n = 5). The proposed method was validated by analysis of two standard reference materials (SRMs) and various real samples, and satisfactory results were obtained.

Determination of vitamin E and carotenoid pigments by high performance liquid chromatography in shell of Chionoecetes opilio.

PubMed

Vilasoa-Martínez, María; Calaza-Ramos, Carina; López-Hernández, Julia; Lage-Yusty, María Asunción; Losada, Perfecto Paseiro; Rodríguez-Bernaldo de Quirós, Ana

2008-06-09

This study reports the optimization of a method for the determination of vitamin E and carotenoids in shells of Chionoecetes opilio samples by online HPLC coupled with UV-vis and fluorescence detectors. The carotenoids were determined with diode-array detector (lambda 450 nm) and vitamin E with fluorescence detection (lambda(ex) 288, lambda(em) 331 nm). Two extractions methods were compared, saponification followed by an extraction step and a simple extraction with acetone. The last one was selected because allows to determine all compounds. Linearity, precisions and recoveries achieved for all compounds were satisfactory. Mean concentrations (mg per 100 g dry weight) were; 23.3 for vitamin E, 9.49 for astaxanthin and 0.2 mg for beta-carotene.

Biofabrication of Ag nanoparticles using Moringa oleifera leaf extract and their antimicrobial activity

PubMed Central

Prasad, TNVKV; Elumalai, EK

2011-01-01

Objective To formulate a simple rapid procedure for bioreduction of silver nanoparticles using aqueous leaves extract of Moringa oleifera (M. oleifera). Methods 10 mL of leaf extract was mixed to 90 mL of 1 mM aqueous of AgNO3 and was heated at 60 - 80 °C for 20 min. A change from brown to reddish color was observed. Characterization using UV-Vis spectrophotometry, Transmission Electron Microscopy (TEM) was performed. Results TEM showed the formation of silver nanoparticles with an average size of 57 nm. Conclusions M. oleifera demonstrates strong potential for synthesis of silver nanoparticles by rapid reduction of silver ions (Ag+ to Ag0). Biological methods are good competents for the chemical procedures, which are eco-friendly and convenient. PMID:23569809

A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry method for the determination of dienogest in human plasma and its pharmacokinetic applications under fasting.

PubMed

Pallapothu, Leela Mohan Kumar; Batta, Neelima; Pigili, Ravi Kumar; Yejella, Rajendra Prasad

2015-02-01

A simple, rapid and sensitive analytical method using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) detection with positive ion electrospray ionization was developed for the determination of dienogest in human K2 EDTA plasma using levonorgestrel d6 as an internal standard (IS). Dienogest and IS were extracted from human plasma using simple liquid-liquid extraction. Chromatographic separation was achieved on a Zorbax XDB-Phenyl column (4.6 × 75 mm, 3.5 µm) under isocratic conditions using acetonitrile-5 mm ammonium acetate (70:30, v/v) at a flow rate of 0.60 mL/min. The protonated precursor to product ion transitions monitored for dienogest and IS were at m/z 312.30 → 135.30 and 319.00 → 251.30, respectively. The method was validated with a linearity range of 1.003-200.896 ng/mL having a total analysis time for each chromatograph of 3.0 min. The method has shown tremendous reproducibility with intra- and inter-day precision (coefficient of variation) <3.97 and 6.10%, respectively, and accuracy within ±4.0% of nominal values. The validated method was applied to a pharmacokinetic study in human plasma samples generated after administration of a single oral dose of 2.0 mg dienogest tablets to healthy female volunteers and was proved to be highly reliable for the analysis of clinical samples. Copyright © 2014 John Wiley & Sons, Ltd.

[Study on extracting and separating curcuminoids from Curcuma longa rhizome using ultrasound strengthen by microemulsion].

PubMed

Yue, Chun-Hua; Zheng, Li-Tao; Guo, Qi-Ming; Li, Kun-Ping

2014-05-01

To establish a new method for the extraction and separation of curcuminoids from Curcuma longa rhizome by cloud-point preconcentration using microemulsions as solvent. The spectrophotometry was used to detect the solubility of curcumin in different oil phase, emulsifier and auxiliary emulsifier, and the microemulsion prescription was used for false three-phase figure optimization. The extraction process was optimized by uniform experiment design. The curcuminoids were separated from microemulsion extract by cloud-point preconcentration. Oil phase was oleic acid ethyl ester; Emulsifier was OP emulsifier; Auxiliary emulsifier was polyethylene glycol(peg) 400; The quantity of emulsifier to auxiliary emulsifier was the ratio of 5: 1; Microemulsion prescription was water-oleic acid ethyl ester-mixed emulsifier (0.45:0.1:0.45). The optimum extraction process was: time for 12.5 min, temperature of 52 degrees C, power of 360 W, frequency of 400 kHz, and the liquid-solid ratio of 40:1. The extraction rate of curcuminoids was 92.17% and 86.85% in microemulsion and oil phase, respectively. Curcuminoids is soluble in this microemulsion prescription with good extraction rate. This method is simple and suitable for curcuminoids extraction from Curcuma longa rhizome.

Recovery of precious metals from space

NASA Technical Reports Server (NTRS)

Freiser, Henry

1991-01-01

The overall objective is to develop efficient and economical separation and recovery methods for the platinum group and other precious metals. The separation of Pd(II) from Pt(II), Ir(III), and Rh(III) with trioctylphosphine oxide (TOPO) in heptane using centrifugal partition chromatography (CPC) was investigated. Activities to achieve this objective focussed on selection and evaluation of extraction systems for the PGM and modification of selected systems for multistage operation with a view to scaling up to desired macro levels. On the basis of preliminary evaluation of a series of simple metal complexing agents and chelating agents, the TOPO in heptane was selected as a likely system for isolating of Pd(II) and Pt(II) from the other PGM. A multistage apparatus capable of configuration as a simple rugged device, a centrifugal partition chromatograph (CPC), was shown to be effective. The extraction of Pd(II) was studied by CPC and batch solvent extraction. The distribution ratios for Pd(II) determined by both methods agree well. In low HCl concentrations (less than 0.1 M), the extracted species was PdCl2.(TOPO)2, irrespective of the chloride concentration, while at acid concentrations above 0.1 M, the Pd was extracted as the ion pair, 2(TOPO.H+).(PdCl4)2-. Base line separation of Pd(II) and Pt(II) in CPC was obtained under a variety of chloride and HCl concentration. It was demonstrated that the efficiency of CPC for metal separation was limited by chemical kinetic factors rather than instrumental factors, strongly suggesting that dramatic improvements can be achieved by studying reaction kinetics of formation and dissociation of the extractable metal complex.

Extended morphological processing: a practical method for automatic spot detection of biological markers from microscopic images.

PubMed

Kimori, Yoshitaka; Baba, Norio; Morone, Nobuhiro

2010-07-08

A reliable extraction technique for resolving multiple spots in light or electron microscopic images is essential in investigations of the spatial distribution and dynamics of specific proteins inside cells and tissues. Currently, automatic spot extraction and characterization in complex microscopic images poses many challenges to conventional image processing methods. A new method to extract closely located, small target spots from biological images is proposed. This method starts with a simple but practical operation based on the extended morphological top-hat transformation to subtract an uneven background. The core of our novel approach is the following: first, the original image is rotated in an arbitrary direction and each rotated image is opened with a single straight line-segment structuring element. Second, the opened images are unified and then subtracted from the original image. To evaluate these procedures, model images of simulated spots with closely located targets were created and the efficacy of our method was compared to that of conventional morphological filtering methods. The results showed the better performance of our method. The spots of real microscope images can be quantified to confirm that the method is applicable in a given practice. Our method achieved effective spot extraction under various image conditions, including aggregated target spots, poor signal-to-noise ratio, and large variations in the background intensity. Furthermore, it has no restrictions with respect to the shape of the extracted spots. The features of our method allow its broad application in biological and biomedical image information analysis.

Simple and rapid quantification of brominated vegetable oil in commercial soft drinks by LC–MS

PubMed Central

Chitranshi, Priyanka; da Costa, Gonçalo Gamboa

2016-01-01

We report here a simple and rapid method for the quantification of brominated vegetable oil (BVO) in soft drinks based upon liquid chromatography–electrospray ionization mass spectrometry. Unlike previously reported methods, this novel method does not require hydrolysis, extraction or derivatization steps, but rather a simple “dilute and shoot” sample preparation. The quantification is conducted by mass spectrometry in selected ion recording mode and a single point standard addition procedure. The method was validated in the range of 5–25 μg/mL BVO, encompassing the legal limit of 15 μg/mL established by the US FDA for fruit-flavored beverages in the US market. The method was characterized by excellent intra- and inter-assay accuracy (97.3–103.4%) and very low imprecision [0.5–3.6% (RSD)]. The direct nature of the quantification, simplicity, and excellent statistical performance of this methodology constitute clear advantages in relation to previously published methods for the analysis of BVO in soft drinks. PMID:27451219

One-step extraction and quantitation of toxic alcohols and ethylene glycol in plasma by capillary gas chromatography (GC) with flame ionization detection (FID).

PubMed

Orton, Dennis J; Boyd, Jessica M; Affleck, Darlene; Duce, Donna; Walsh, Warren; Seiden-Long, Isolde

2016-01-01

Clinical analysis of volatile alcohols (i.e. methanol, ethanol, isopropanol, and metabolite acetone) and ethylene glycol (EG) generally employs separate gas chromatography (GC) methods for analysis. Here, a method for combined analysis of volatile alcohols and EG is described. Volatile alcohols and EG were extracted with 2:1 (v:v) acetonitrile containing internal standards (IS) 1,2 butanediol (for EG) and n-propanol (for alcohols). Samples were analyzed on an Agilent 6890 GC FID. The method was evaluated for precision, accuracy, reproducibility, linearity, selectivity and limit of quantitation (LOQ), followed by correlation to existing GC methods using patient samples, Bio-Rad QC, and in-house prepared QC material. Inter-day precision was from 6.5-11.3% CV, and linearity was verified from down to 0.6mmol/L up to 150mmol/L for each analyte. The method showed good recovery (~100%) and the LOQ was calculated to be between 0.25 and 0.44mmol/L. Patient correlation against current GC methods showed good agreement (slopes from 1.03-1.12, and y-intercepts from 0 to 0.85mmol/L; R(2)>0.98; N=35). Carryover was negligible for volatile alcohols in the measuring range, and of the potential interferences tested, only toluene and 1,3 propanediol interfered. The method was able to resolve 2,3 butanediol, diethylene glycol, and propylene glycol in addition to the peaks quantified. Here we describe a simple procedure for simultaneous analysis of EG and volatile alcohols that comes at low cost and with a simple liquid-liquid extraction requiring no derivitization to obtain adequate sensitivity for clinical specimens. Copyright © 2015 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

A Semantic Graph Query Language

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

Kaplan, I L

2006-10-16

Semantic graphs can be used to organize large amounts of information from a number of sources into one unified structure. A semantic query language provides a foundation for extracting information from the semantic graph. The graph query language described here provides a simple, powerful method for querying semantic graphs.

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography

PubMed Central

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-01-01

Purpose: To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). Methods: The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min−1 at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. Results: The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. Conclusion: This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants. PMID:26819933

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Imprinted magnetic graphene oxide for the mini-solid phase extraction of Eu (III) from coal mine area

NASA Astrophysics Data System (ADS)

Patra, Santanu; Roy, Ekta; Madhuri, Rashmi; Sharma, Prashant K.

2017-05-01

The present work represents the preparation of imprinted magnetic reduced graphene oxide and applied it for the selective removal of Eu (III) from local coal mines area. A simple solid phase extraction method was used for this purpose. The material shows a very high adsorption as well as removal efficiency towards Eu (III), which suggest that the material have potential to be used in future for their real time applications in removal of Eu (III) from complex matrices.

System and method for automated object detection in an image

DOEpatents

Kenyon, Garrett T.; Brumby, Steven P.; George, John S.; Paiton, Dylan M.; Schultz, Peter F.

2015-10-06

A contour/shape detection model may use relatively simple and efficient kernels to detect target edges in an object within an image or video. A co-occurrence probability may be calculated for two or more edge features in an image or video using an object definition. Edge features may be differentiated between in response to measured contextual support, and prominent edge features may be extracted based on the measured contextual support. The object may then be identified based on the extracted prominent edge features.

Enhanced determination of abscisic acid (ABA) and abscisic acid glucose ester (ABA-GE) in Cistus albidus plants by liquid chromatography-mass spectrometry in tandem mode.

PubMed

López-Carbonell, Marta; Gabasa, Marta; Jáuregui, Olga

2009-04-01

An improved, quick and simple method for the extraction and quantification of the phytohormones (+)-abscisic acid (ABA) and its major glucose conjugate, abscisic acid glucose ester (ABA-GE) in plant samples is described. The method includes the addition of deuterium-labeled internal standards to the leaves at the beginning of the extraction for quantification, a simple extraction/centrifugation process and the injection into the liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) system in multiple reaction monitoring mode (MRM). Quality parameters of the method (detection limits, repeatability, reproducibility and linearity) have been studied. The objective of this work is to show the applicability of this method for quantifying the endogenous content of both ABA and ABA-GE in Cistus albidus plants that have been grown during an annual cycle under Mediterranean field conditions. Leaf samples from winter plants have low levels of ABA which increase in spring and summer showing two peaks that corresponded to April and August. These increases are coincident with the high temperature and solar radiation and the low RWC and RH registered along the year. On the other hand, the endogenous levels of ABA-GE increase until maximum values in July just before the ABA content reaches its highest concentration, decreasing in August and during autumn and winter. Our results suggest that the method is useful for quantifying both compounds in this plant material and represents the advantage of a short-time sample preparation with a high accuracy and viability.

[Studies on six heavy metal elements dissolution characteristics of Andrographis herb by ICP-OES].

PubMed

Tang, Rui; Li, Tian-Peng; Gu, Xue-Shi; Li, Yong-Jian; Yang, Yi

2010-02-01

A simple and accurate method for the simultaneous determination of As, Ba, Cd, Cr, Cu and Pb in andrographis herb by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The samples were digested by HNO3-HClO4. The digestion-determination method was evaluated with the relative standard deviations for all these elements between 2.1% and 4.6%, and the recoveries were between 92.0% and 103.2%. The measuring method was proved to be simple, reliable and highly sensitive. The dissolution characteristics of the 6 heavy metal elements in different solvents and with different extraction methods such as refluxing, soaking, and ultrasonic assisted extraction were studied. The experimental results showed that Ba was in the highest concentration followed by Cu and Cr, and the concentration of As, Pb and Cd was relatively lower in the herb. With the increase in ethanol concentration, the dissolution amount of Ba decreased but that of Cu and Cr increased, and the highest concentration of Cd was dissolved in acidic solution. Overall, Cd and Pb were difficult to dissolve out with 85% ethanol refluxing, but As dissolved comparatively more under the same condition. Comparing the extraction methods, the higher concentration of these 6 metals was obtained by refluxing water or alkaline water than that by 85% ethanol maceration. These differences might be related to the existent forms of these six elements in the herb. The determination and study on dissolution characteristics of these elements by using ICP-OES was important for rational using medicinal resources and ensuring the safety of drugs.

Magnetic molecularly imprinted polymer for the selective extraction of quercetagetin from Calendula officinalis extract.

PubMed

Ma, Run-Tian; Shi, Yan-Ping

2015-03-01

A new magnetic molecularly imprinted polymers (MMIPs) for quercetagetin was prepared by surface molecular imprinting method using super paramagnetic core-shell nanoparticle as the supporter. Acrylamide as the functional monomer, ethyleneglycol dimethacrylate as the crosslinker and acetonitrile as the porogen were applied in the preparation process. Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Vibrating sample magnetometer (VSM) were applied to characterize the MMIPs, and High performance liquid chromatography (HPLC) was utilized to analyze the target analytes. The selectivity of quercetagetin MMIPs was evaluated according to their recognition to template and its analogues. Excellent binding for quercetagetin was observed in MMIPs adsorption experiment, and the adsorption isotherm models analysis showed that the homogeneous binding sites were distributed on the surface of the MMIPs. The MMIPs were employed as adsorbents in solid phase extraction for the determination of quercetagetin in Calendula officinalis extracts. Furthermore, this method is fast, simple and could fulfill the determination and extraction of quercetagetin from herbal extract. Copyright © 2014 Elsevier B.V. All rights reserved.

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Extraction of Fucoxanthin from Raw Macroalgae excluding Drying and Cell Wall Disruption by Liquefied Dimethyl Ether

PubMed Central

Kanda, Hideki; Kamo, Yuichi; Machmudah, Siti; Wahyudiono; Goto, Motonobu

2014-01-01

Macroalgae are one of potential sources for carotenoids, such as fucoxanthin, which are consumed by humans and animals. This carotenoid has been applied in both the pharmaceutical and food industries. In this study, extraction of fucoxanthin from wet brown seaweed Undaria pinnatifida (water content was 93.2%) was carried out with a simple method using liquefied dimethyl ether (DME) as an extractant in semi-continuous flow-type system. The extraction temperature and absolute pressure were 25 °C and 0.59 MPa, respectively. The liquefied DME was passed through the extractor that filled by U. pinnatifida at different time intervals. The time of experiment was only 43 min. The amount of fucoxanthin could approach to 390 μg/g dry of wet U. pinnatifida when the amount of DME used was 286 g. Compared with ethanol Soxhlet and supercritical CO2 extraction, which includes drying and cell disruption, the result was quite high. Thus, DME extraction process appears to be a good method for fucoxanthin recovery from U. pinnatifida with improved yields. PMID:24796299

Investigation of cloud point extraction for the analysis of metallic nanoparticles in a soil matrix

PubMed Central

Hadri, Hind El; Hackley, Vincent A.

2017-01-01

The characterization of manufactured nanoparticles (MNPs) in environmental samples is necessary to assess their behavior, fate and potential toxicity. Several techniques are available, but the limit of detection (LOD) is often too high for environmentally relevant concentrations. Therefore, pre-concentration of MNPs is an important component in the sample preparation step, in order to apply analytical tools with a LOD higher than the ng kg−1 level. The objective of this study was to explore cloud point extraction (CPE) as a viable method to pre-concentrate gold nanoparticles (AuNPs), as a model MNP, spiked into a soil extract matrix. To that end, different extraction conditions and surface coatings were evaluated in a simple matrix. The CPE method was then applied to soil extract samples spiked with AuNPs. Total gold, determined by inductively coupled plasma mass spectrometry (ICP-MS) following acid digestion, yielded a recovery greater than 90 %. The first known application of single particle ICP-MS and asymmetric flow field-flow fractionation to evaluate the preservation of the AuNP physical state following CPE extraction is demonstrated. PMID:28507763

Analysis of carbendazim, benomyl, thiophanate methyl and 2,4-dichlorophenoxyacetic acid in fruits and vegetables after supercritical fluid extraction.

PubMed

Anastassiades, M; Schwack, W

1998-10-30

Simple methods for the analysis of carbendazim, benomyl and thiophanate methyl in fruits and vegetables and of 2,4-D in citrus fruits are presented. Sample preparation involves supercritical fluid extraction with carbon dioxide and further analysis is performed without any additional clean-up by GC-MS after derivatisation or directly by HPLC-diode array detection. The SFE methods presented are clearly faster and more cost effective than traditional solvent based approaches. The recoveries, detection limits and repeatabilities achieved, meet the needs of tolerance level monitoring of these compounds in fruits and vegetables.

Analysis of flavor compounds by GC/MS after liquid-liquid extraction from fruit juices

NASA Astrophysics Data System (ADS)

Tuşa, F. D.; Moldovan, Z.; Schmutzer, G.; Magdaş, D. A.; Dehelean, A.; Vlassa, M.

2012-02-01

In this work we describe a rapid method for analysis of volatile profiles of several commercial fruit juices using GC/MS instrument after liquid-liquid extraction. Volatile flavor compounds have been identified based on mass spectrum obtained in EI mode. This method allows to analyses a wide range of flavor compounds (esters, aldehydes, alcohols, terpenoids) the procedure was rapid, simple and inexpensive. Moreover, by means of volatile compounds it could be possible to distinguish between juices of organic and conventional production and those with flavorings addition. More of 20 compounds were identified and quantified as relative chromatogram area taken on larges ion in mass spectrum.

The Amount and Preferred Orientation of Simple-shear in a Deformation Tensor: Implications for Detecting Shear Zones and Faults with GPS

NASA Astrophysics Data System (ADS)

Johnson, A. M.; Griffiths, J. H.

2007-05-01

At the 2005 Fall Meeting of the American Geophysical Union, Griffiths and Johnson [2005] introduced a method of extracting from the deformation-gradient (and velocity-gradient) tensor the amount and preferred orientation of simple-shear associated with 2-D shear zones and faults. Noting the 2-D is important because the shear zones and faults in Griffiths and Johnson [2005] were assumed non-dilatant and infinitely long, ignoring the scissors- like action along strike associated with shear zones and faults of finite length. Because shear zones and faults can dilate (and contract) normal to their walls and can have a scissors-like action associated with twisting about an axis normal to their walls, the more general method of detecting simple-shear is introduced and called MODES "method of detecting simple-shear." MODES can thus extract from the deformation-gradient (and velocity- gradient) tensor the amount and preferred orientation of simple-shear associated with 3-D shear zones and faults near or far from the Earth's surface, providing improvements and extensions to existing analytical methods used in active tectonics studies, especially strain analysis and dislocation theory. The derivation of MODES is based on one definition and two assumptions: by definition, simple-shear deformation becomes localized in some way; by assumption, the twirl within the deformation-gradient (or the spin within the velocity-gradient) is due to a combination of simple-shear and twist, and coupled with the simple- shear and twist is a dilatation of the walls of shear zones and faults. The preferred orientation is thus the orientation of the plane containing the simple-shear and satisfying the mechanical and kinematical boundary conditions. Results from a MODES analysis are illustrated by means of a three-dimensional diagram, the cricket- ball, which is reminiscent of the seismologist's "beach ball." In this poster, we present the underlying theory of MODES and illustrate how it works by analyzing the three- dimensional displacements measured with the Global Positioning System across the 1999 Chi-Chi earthquake ground rupture in Taiwan. In contrast to the deformation zone in the upper several meters of the ground below the surface detected by Yu et al. [2001], MODES determines the orientation and direction of shift of a shear zone representing the earthquake fault within the upper several hundred or thousand meters of ground below the surface. Thus, one value of the MODES analysis in this case is to provide boundary conditions for dislocation solutions for the subsurface shape of the main rupture during the earthquake.

[Extraction, isolation and purification for ginkgolide B].

PubMed

Zhang, Chenfeng; Li, Minghui; Tang, Yun; Zhang, Yanhai; Shi, Min; Sheng, Longsheng

2010-08-01

To establish a simple extraction, isolation and purification method for ginkgolide B from ginkgo leaf. The optimum conditions of extraction, isolation and purification were studied by taking the transfer rate of ginkgolide B as index. Ginkgo leaf was extracted with 70% ethanol for three times, the extracts were concentrated to remove ethanol and diluted by water till the crude drug density reached 0.1 g x mL(-1). The dilution was adsorbed with HPD-450 macroporous resin. The impurities were eluted with 20% ethanol and ginkgolide B was eluted with 80% ethanol. Then the 80% ethanol eluant was concentrated and crystallized. Finally the crude crystals were recrystallized with isopropanol. The purity of the ginkgolide B recrystallization was 95%. The process was stable and easy to operate, which was suited to industrialized production.

A Simple and Quick Method for the Determination of Pesticides in Environmental Water by HF-LPME-GC/MS

PubMed Central

Paulo, Breno P.; Paiva, Maria José N.

2016-01-01

This paper describes a simple and quick method for sampling and also for carrying out the preconcentration of pesticides in environmental water matrices using two-phased hollow fiber liquid phase microextraction (HF-LPME). Factors such as extraction mode, time, solvents, agitation, and salt addition were investigated in order to validate the LPME method. The following conditions were selected: 6 cm of polypropylene hollow fiber, ethyl octanoate as an acceptor phase, and extraction during 30 min under stirring at 200 rpm. The optimized method showed good linearity in the range of 0.14 to 200.00 μg L−1; the determination coefficient (R 2) was in the range of 0.9807–0.9990. The LOD ranged from 0.04 μg L−1 to 0.44 μg L−1, and LOQ ranged from 0.14 μg L−1 to 1.69 μg L−1. The recovery ranged from 85.17% to 114.73%. The method was applied to the analyses of pesticides in three environmental water samples (a spring and few streams) collected in a rural area from the state of Minas Gerais, Brazil. PMID:27774336

A simple and accurate HPLC method for fecal bile acid profile in healthy and cirrhotic subjects: validation by GC-MS and LC-MS[S

PubMed Central

Kakiyama, Genta; Muto, Akina; Takei, Hajime; Nittono, Hiroshi; Murai, Tsuyoshi; Kurosawa, Takao; Hofmann, Alan F.; Pandak, William M.; Bajaj, Jasmohan S.

2014-01-01

We have developed a simple and accurate HPLC method for measurement of fecal bile acids using phenacyl derivatives of unconjugated bile acids, and applied it to the measurement of fecal bile acids in cirrhotic patients. The HPLC method has the following steps: 1) lyophilization of the stool sample; 2) reconstitution in buffer and enzymatic deconjugation using cholylglycine hydrolase/sulfatase; 3) incubation with 0.1 N NaOH in 50% isopropanol at 60°C to hydrolyze esterified bile acids; 4) extraction of bile acids from particulate material using 0.1 N NaOH; 5) isolation of deconjugated bile acids by solid phase extraction; 6) formation of phenacyl esters by derivatization using phenacyl bromide; and 7) HPLC separation measuring eluted peaks at 254 nm. The method was validated by showing that results obtained by HPLC agreed with those obtained by LC-MS/MS and GC-MS. We then applied the method to measuring total fecal bile acid (concentration) and bile acid profile in samples from 38 patients with cirrhosis (17 early, 21 advanced) and 10 healthy subjects. Bile acid concentrations were significantly lower in patients with advanced cirrhosis, suggesting impaired bile acid synthesis. PMID:24627129

DNA recovery from soils of diverse composition.

PubMed

Zhou, J; Bruns, M A; Tiedje, J M

1996-02-01

A simple, rapid method for bacterial lysis and direct extraction of DNA from soils with minimal shearing was developed to address the risk of chimera formation from small template DNA during subsequent PCR. The method was based on lysis with a high-salt extraction buffer (1.5 M NaCl) and extended heating (2 to 3 h) of the soil suspension in the presence of sodium dodecyl sulfate (SDS), hexadecyltrimethylammonium bromide, and proteinase K. The extraction method required 6 h and was tested on eight soils differing in organic carbon, clay content, and pH, including ones from which DNA extraction is difficult. The DNA fragment size in crude extracts from all soils was > 23 kb. Preliminary trials indicated that DNA recovery from two soils seeded with gram-negative bacteria was 92 to 99%. When the method was tested on all eight unseeded soils, microscopic examination of indigenous bacteria in soil pellets before and after extraction showed variable cell lysis efficiency (26 to 92%). Crude DNA yields from the eight soils ranged from 2.5 to 26.9 micrograms of DNA g-1, and these were positively correlated with the organic carbon content in the soil (r = 0.73). DNA yields from gram-positive bacteria from pure cultures were two to six times higher when the high-salt-SDS-heat method was combined with mortar-and-pestle grinding and freeze-thawing, and most DNA recovered was of high molecular weight. Four methods for purifying crude DNA were also evaluated for percent recovery, fragment size, speed, enzyme restriction, PCR amplification, and DNA-DNA hybridization. In general, all methods produced DNA pure enough for PCR amplification. Since soil type and microbial community characteristics will influence DNA recovery, this study provides guidance for choosing appropriate extraction and purification methods on the basis of experimental goals.

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography.

PubMed

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-11-01

To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min(-1) at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants.

Considering context: reliable entity networks through contextual relationship extraction

NASA Astrophysics Data System (ADS)

David, Peter; Hawes, Timothy; Hansen, Nichole; Nolan, James J.

2016-05-01

Existing information extraction techniques can only partially address the problem of exploiting unreadable-large amounts text. When discussion of events and relationships is limited to simple, past-tense, factual descriptions of events, current NLP-based systems can identify events and relationships and extract a limited amount of additional information. But the simple subset of available information that existing tools can extract from text is only useful to a small set of users and problems. Automated systems need to find and separate information based on what is threatened or planned to occur, has occurred in the past, or could potentially occur. We address the problem of advanced event and relationship extraction with our event and relationship attribute recognition system, which labels generic, planned, recurring, and potential events. The approach is based on a combination of new machine learning methods, novel linguistic features, and crowd-sourced labeling. The attribute labeler closes the gap between structured event and relationship models and the complicated and nuanced language that people use to describe them. Our operational-quality event and relationship attribute labeler enables Warfighters and analysts to more thoroughly exploit information in unstructured text. This is made possible through 1) More precise event and relationship interpretation, 2) More detailed information about extracted events and relationships, and 3) More reliable and informative entity networks that acknowledge the different attributes of entity-entity relationships.

Determination of the Effect of Various Modes of Cooking on the Vitamin C Content of a Common Food, Green Pepper: An Introductory Biochemistry Experiment.

ERIC Educational Resources Information Center

Johnson, Eric R.

1988-01-01

Describes a laboratory experiment that measures the amount of ascorbic acid destroyed by food preparation methods (boiling and steaming). Points out that aqueous extracts of cooked green pepper samples can be analyzed for ascorbic acid by a relatively simple redox titration. Lists experimental procedure for four methods of preparation. (MVL)

Validated method for the analysis of goji berry, a rich source of zeaxanthin dipalmitate.

PubMed

Karioti, Anastasia; Bergonzi, Maria Camilla; Vincieri, Franco F; Bilia, Anna Rita

2014-12-31

In the present study an HPLC-DAD method was developed for the determination of the main carotenoid, zeaxanthin dipalmitate, in the fruits of Lycium barbarum. The aim was to develop and optimize an extraction protocol to allow fast, exhaustive, and repeatable extraction, suitable for labile carotenoid content. Use of liquid N2 allowed the grinding of the fruit. A step of ultrasonication with water removed efficiently the polysaccharides and enabled the exhaustive extraction of carotenoids by hexane/acetone 50:50. The assay was fast and simple and permitted the quality control of a large number of commercial samples including fruits, juices, and a jam. The HPLC method was validated according to ICH guidelines and satisfied the requirements. Finally, the overall method was validated for precision (% RSD ranging between 3.81 and 4.13) and accuracy at three concentration levels. The recovery was between 94 and 107% with RSD values <2%, within the acceptable limits, especially if the difficulty of the matrix is taken into consideration.

Optimization and Validation of Thermal Desorption Gas Chromatography-Mass Spectrometry for the Determination of Polycyclic Aromatic Hydrocarbons in Ambient Air

PubMed Central

Durana, Nieves; García, José Antonio; Gómez, María Carmen; Alonso, Lucio

2018-01-01

Thermal desorption (TD) coupled with gas chromatography/mass spectrometry (TD-GC/MS) is a simple alternative that overcomes the main drawbacks of the solvent extraction-based method: long extraction times, high sample manipulation, and large amounts of solvent waste. This work describes the optimization of TD-GC/MS for the measurement of airborne polycyclic aromatic hydrocarbons (PAHs) in particulate phase. The performance of the method was tested by Standard Reference Material (SRM) 1649b urban dust and compared with the conventional method (Soxhlet extraction-GC/MS), showing a better recovery (mean of 97%), precision (mean of 12%), and accuracy (±25%) for the determination of 14 EPA PAHs. Furthermore, other 15 nonpriority PAHs were identified and quantified using their relative response factors (RRFs). Finally, the proposed method was successfully applied for the quantification of PAHs in real 8 h-samples (PM10), demonstrating its capability for determination of these compounds in short-term monitoring. PMID:29854561

Direct analysis of organic priority pollutants by IMS

NASA Technical Reports Server (NTRS)

Giam, C. S.; Reed, G. E.; Holliday, T. L.; Chang, L.; Rhodes, B. J.

1995-01-01

Many routine methods for monitoring of trace amounts of atmospheric organic pollutants consist of several steps. Typical steps are: (1) collection of the air sample; (2) trapping of organics from the sample; (3) extraction of the trapped organics; and (4) identification of the organics in the extract by GC (gas chromatography), HPLC (High Performance Liquid Chromatography), or MS (Mass Spectrometry). These methods are often cumbersome and time consuming. A simple and fast method for monitoring atmospheric organics using an IMS (Ion Mobility Spectrometer) is proposed. This method has a short sampling time and does not require extraction of the organics since the sample is placed directly in the IMS. The purpose of this study was to determine the responses in the IMS to organic 'priority pollutants'. Priority pollutants including representative polycyclic aromatic hydrocarbons (PAHs), phthalates, phenols, chlorinated pesticides, and polychlorinated biphenyls (PCB's) were analyzed in both the positive and negative detection mode at ambient atmospheric pressure. Detection mode and amount detected are presented.

A Fast Liquid Chromatography Tandem Mass Spectrometric Analysis of PETN (Pentaerythritol Tetranitrate), RDX (3,5-Trinitro-1,3,5-triazacyclohexane) and HMX (Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) in Soil, Utilizing a Simple Ultrasonic-Assisted Extraction with Minimum Solvent.

PubMed

Anilanmert, Beril; Aydin, Muhammet; Apak, Resat; Avci, Gülfidan Yenel; Cengiz, Salih

2016-01-01

Direct analyses of explosives in soil using liquid chromatography tandem mass spectrometry (LC-MS/MS) methods are very limited in the literature and require complex procedures or relatively high amount of solvent. A simple and rapid method was developed for the determination of pentaerythritol tetranitrate (PETN), 3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), which are among the explosives used in terrorist attacks. A one-step extraction method for 1.00 g soil with 2.00 mL acetonitrile, and a 8-min LC-MS/MS method was developed. The detection limits for PETN, RDX and HMX were 5.2, 8.5 and 3.4 ng/g and quantitation limits were 10.0, 24.5, 6.0 ng/g. The intermediate precisions and Horwitz Ratio's were between 4.10 - 13.26% and 0.24 - 0.98, in order. This method was applied to a model post-blast debris collected from an artificial explosion and real samples collected after a terrorist attack in Istanbul. The method is easy and fast and requires less solvent use than other methods.

Rapid Solid-Liquid Dynamic Extraction (RSLDE): a New Rapid and Greener Method for Extracting Two Steviol Glycosides (Stevioside and Rebaudioside A) from Stevia Leaves.

PubMed

Gallo, Monica; Vitulano, Manuela; Andolfi, Anna; DellaGreca, Marina; Conte, Esterina; Ciaravolo, Martina; Naviglio, Daniele

2017-06-01

Stevioside and rebaudioside A are the main diterpene glycosides present in the leaves of the Stevia rebaudiana plant, which is used in the production of foods and low-calorie beverages. The difficulties associated with their extraction and purification are currently a problem for the food processing industries. The objective of this study was to develop an effective and economically viable method to obtain a high-quality product while trying to overcome the disadvantages derived from the conventional transformation processes. For this reason, extractions were carried out using a conventional maceration (CM) and a cyclically pressurized extraction known as rapid solid-liquid dynamic extraction (RSLDE) by the Naviglio extractor (NE). After only 20 min of extraction using the NE, a quantity of rebaudioside A and stevioside equal to 1197.8 and 413.6 mg/L was obtained, respectively, while for the CM, the optimum time was 90 min. From the results, it can be stated that the extraction process by NE and its subsequent purification developed in this study is a simple, economical, environmentally friendly method for producing steviol glycosides. Therefore, this method constitutes a valid alternative to conventional extraction by reducing the extraction time and the consumption of toxic solvents and favouring the use of the extracted metabolites as food additives and/or nutraceuticals. As an added value and of local interest, the experiment was carried out on stevia leaves from the Benevento area (Italy), where a high content of rebaudioside A was observed, which exhibits a sweet taste compared to stevioside, which has a significant bitter aftertaste.

OPPORTUNISTIC ASPERGILLUS PATHOGENS MEASURED IN HOME AND HOSPITAL TAP WATER BY MOLD SPECIFIC QUANTITATIVE PCR (MSQPCR)

EPA Science Inventory

Opportunistic fungal pathogens are a concern because of the increasing number of immunocompromised patients. The goal of this research was to test a simple extraction method and rapid quantitative PCR (QPCR) measurement of the occurrence of potential pathogens, Aspergillus fumiga...

The Study of Residential Areas Extraction Based on GF-3 Texture Image Segmentation

NASA Astrophysics Data System (ADS)

Shao, G.; Luo, H.; Tao, X.; Ling, Z.; Huang, Y.

2018-04-01

The study chooses the standard stripe and dual polarization SAR images of GF-3 as the basic data. Residential areas extraction processes and methods based upon GF-3 images texture segmentation are compared and analyzed. GF-3 images processes include radiometric calibration, complex data conversion, multi-look processing, images filtering, and then conducting suitability analysis for different images filtering methods, the filtering result show that the filtering method of Kuan is efficient for extracting residential areas, then, we calculated and analyzed the texture feature vectors using the GLCM (the Gary Level Co-occurrence Matrix), texture feature vectors include the moving window size, step size and angle, the result show that window size is 11*11, step is 1, and angle is 0°, which is effective and optimal for the residential areas extracting. And with the FNEA (Fractal Net Evolution Approach), we segmented the GLCM texture images, and extracted the residential areas by threshold setting. The result of residential areas extraction verified and assessed by confusion matrix. Overall accuracy is 0.897, kappa is 0.881, and then we extracted the residential areas by SVM classification based on GF-3 images, the overall accuracy is less 0.09 than the accuracy of extraction method based on GF-3 Texture Image Segmentation. We reached the conclusion that residential areas extraction based on GF-3 SAR texture image multi-scale segmentation is simple and highly accurate. although, it is difficult to obtain multi-spectrum remote sensing image in southern China, in cloudy and rainy weather throughout the year, this paper has certain reference significance.

Determination of triazine herbicides in fresh vegetables by dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction high performance liquid chromatography.

PubMed

Wu, Lijie; Hu, Mingzhu; Li, Zhanchao; Song, Ying; Yu, Cui; Zhang, Yupu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-02-01

A novel extraction method, dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction, was developed for the determination of triazine herbicides, including desmetryn, terbumeton, propazine, terbuthylazine, dimethametryn, and dipropetryn in fresh vegetable samples by high performance liquid chromatography (HPLC). In the developed method, 120 μL of 1-butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) was added to 10 mL of aqueous solution containing 0.3 g of NaCl to obtained the extraction solvent. Six triazines could be extracted completely within 4 min by the present method. Then, [NH4][PF6] was added into the extract to form a water-insoluble ionic liquid [C4MIM][PF6] via a simple metathesis reaction, and the analytes were enriched into the ionic liquid phase. After centrifugation and dilution with acetonitrile, the resulting solution was analyzed directly by HPLC. The effects of some experimental parameters, including type and volume of ionic liquid, volume of extraction solvent, amount of ion-pairing agent [NH4][PF6], salt concentration, microwave power, and flow rate of extraction solvent on the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 2.50-250.00 μg kg(-1), with the correlation coefficients ranging from 0.9989 to 0.9999. When the present method was applied to the analysis of vegetable samples, satisfactory recoveries were obtained in the range of 76.8%-106.9%, and relative standard deviations were lower than 9.8%.

Development of an enzyme-linked immunosorbent assay for seven sulfonamide residues and investigation of matrix effects from different food samples.

PubMed

Zhang, Hongyan; Wang, Lei; Zhang, Yan; Fang, Guozhen; Zheng, Wenjie; Wang, Shuo

2007-03-21

Direct competitive enzyme-linked immunosorbent assays (ELISA) were developed to detect a broad range of sulfonamides in various matrices. Screening for this class of antibiotics in pig muscle, chicken muscle, fish, and egg extracts was accomplished by simple, rapid extraction methods carried out with only phosphate-buffered saline (PBS) buffer. Twenty milliliters of extract solution was added to 4 g of sample to extract the sulfonamide residues, and sample extracts diluted with assay buffer were directly analyzed by ELISA; matrix effects could be avoided with 1:5 dilution of pig muscle, chicken muscle, and egg extracts with PBS and 1:5 dilution of fish extract with 1% bovine serum albumin (BSA)-PBS. For liver sample, the extraction method was a little more complicated; 2 g of sample was added to 20 mL of ethanol, mixed, and then centrifuged. The solvent of 10 mL of the upper liquid was removed, and the residues were dissolved in 10 mL of PBS and then filtered; the filtrate was diluted two-fold with 0.5% BSA-PBS for ELISA. These common methods were able to detect seven sulfonamide residues such as sulfisozole, sulfathiazole, sufameter, sulfamethoxypyridazine, sulfapyridine, sulfamethizole, and sulfachlorpyridazine in pig muscle, liver, chicken muscle, egg, and fish. The assay's detection limits for these compounds were less than 100 microg kg-1. Various extraction methods were tested, and the average recovery (n=3) of 100 microg kg-1 for the matrices was found to range from 77.3 to 123.7%.

Flow injection spectrophotometry using natural reagent from Morinda citrifolia root for determination of aluminium in tea.

PubMed

Tontrong, Sopa; Khonyoung, Supada; Jakmunee, Jaroon

2012-05-01

A flow injection (FI) spectrophotometric method with using natural reagent extracted from Morinda citrifolia root has been developed for determination of aluminium. The extract contained anthraquinone compounds which could react with Al(3+) to form reddish complexes which had maximum absorption wavelength at 499.0nm. The extract could be used as a reagent in FI system without further purification to obtain pure compound. A sensitive method for determination of aluminium in concentration range of 0.1-1.0mgL(-1), with detection limit of 0.05mgL(-1) was achieved. Relative standard deviations of 1.2% and 1.7% were obtained for the determination of 0.1 and 0.6mgL(-1) Al(3+) (n=11). Sample throughput of 35h(-1) was achieved with the consumption of 3mL each of carrier and reagent solutions per injection. The developed method was successfully applied to tea samples, validated by the FAAS standard method. The method is simple, fast, economical and could be classified as a greener analytical method. Copyright © 2011 Elsevier Ltd. All rights reserved.

[Determination of acacetin in Xiangjuganmao Keli (no sweet) by HPLC].

PubMed

Bian, Jia-Hong; Qian, Kun; Xu, Xiang; Shen, Jun

2006-11-01

To establish a method for the determination of acacetin in Xiangjuganmao Keli (no sweet). Acacetin in powdered herb was extracted by ultrasonator with methanol and was hydrolyzed with hydrochloric acid. Separation was accomplished on an ODS reversed phase column (5 microm, 4.6 x 250 mm) with a mobile phase of methanol-water-acetic acid(350: 150: 2). The detective wavelength was at 340 nm. The method was accurate, the results were stable and reproducible. The linear range of calibration cure was within the concentration of 2.00 - 10.00 microg/ml (r = 0.9998). The average extraction recovery was 99.9% (n = 6), RSD = 0.41% (n = 6). The method is simple, convenient, sensitive, and reproducible for quality control of Xiangjuganmao Keli (no sweet).

[Optimization of dissolution process for superfine grinding technology on total saponins of Panax ginseng fibrous root by response surface methodology].

PubMed

Zhao, Ya; Lai, Xiao-Pin; Yao, Hai-Yan; Zhao, Ran; Wu, Yi-Na; Li, Geng

2014-03-01

To investigate the effects of superfine comminution extraction technology of ginseng total saponins from Panax ginseng fibrous root, and to make sure the optimal extraction condition. Optimal condition of ginseng total saponins from Panax ginseng fibrous root was based on single factor experiment to study the effects of crushing degree, extraction time, alcohol concentration and extraction temperature on extraction rate. Response surface method was used to investigate three main factors such as superfine comminution time, extraction time and alcohol concentration. The relationship between content of ginseng total saponins in Panax ginseng fibrous root and three factors fitted second degree polynomial models. The optimal extraction condition was 9 min of superfine comminution time, 70% of alcohol, 50 degrees C of extraction temperature and 70 min of extraction time. Under the optimal condition, ginseng total saponins from Panax ginseng fibrous root was average 94. 81%, which was consistent with the predicted value. The optimization of technology is rapid, efficient, simple and stable.

Pipette-tip solid-phase extraction using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a new molecularly imprinted polymer in the determination of avermectins and milbemycins in fruit juice and water samples.

PubMed

Teixeira, Roseane Andrade; Flores, Diego Hernando Ângulo; da Silva, Ricky Cássio Santos; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

2018-10-01

A simple HPLC method was developed for the determination of abamectin (ABA), eprinomectin (EPR), and moxidectin (MOX). Pipette-tip molecularly imprinted polymer solid-phase extraction (PT-MIP-SPE) using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a selective adsorbent material was studied in detail, including the washing solvent, type and volume of eluent, pH, quantity of adsorbent material and sample volume. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, robustness and stability have been assessed and were within the recommended guidelines. The mean extraction recoveries/relative standard deviation for ABA 1b, EPR, ABA 1a and MOX were 98.77 ± 3.82%, 88.19 ± 2.57%, 110.54 ± 1.52% and 100.42 ± 0.59%, respectively. Finally, the results proved that PT-MIP-SPE coupled to HPLC-UV is an economical, simple and easy-to-perform technique, and presented a high potential for extraction of macrocyclic lactones in mineral water and grape and juice samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Evaluation of new natural deep eutectic solvents for the extraction of isoflavones from soy products.

PubMed

Bajkacz, Sylwia; Adamek, Jakub

2017-06-01

Natural deep eutectic solvents (NADESs) are considered to be new, safe solvents in green chemistry that can be widely used in many chemical processes such as extraction or synthesis. In this study, a simple extraction method based on NADES was used for the isolation of isoflavones (daidzin, genistin, genistein, daidzein) from soy products. Seventeen different NADES systems each including two or three components were tested. Multivariate data analysis revealed that NADES based on a 30% solution of choline chloride: citric acid (molar ratio of 1:1) are the most effective systems for the extraction of isoflavones from soy products. After extraction, the analytes were detected and quantified using ultra-high performance liquid chromatography with ultraviolet detection (UHPLC-UV). The proposed NADES extraction procedure achieved enrichment factors up to 598 for isoflavones and the recoveries of the analytes were in the range 64.7-99.2%. The developed NADES extraction procedure and UHPLC-UV determination method was successfully applied for the analysis of isoflavones in soy-containing food samples. The obtained results indicated that new natural deep eutectic solvents could be an alternative to traditional solvents for the extraction of isoflavones and can be used as sustainable and safe extraction media for another applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of methods for extracting DNA from formalin-fixed paraffin sections for nonisotopic PCR.

PubMed

Frank, T S; Svoboda-Newman, S M; Hsi, E D

1996-09-01

DNA was extracted from unstained 5-microns sections of neutral buffered 10% formalin-fixed paraffin-embedded tissue by proteinase K digestion without detergents followed by boiling, proteinase K digestion with ionic detergents with and without phenol chloroform extraction and ethanol precipitation, sonication with proteinase K followed by boiling, or boiling alone. Serial 1:10 dilutions of the extracted DNA were subject to polymerase chain reaction (PCR) amplification of a 255-bp portion of the p53 gene. Digestion with proteinase K without ionic detergents followed by boiling (without phenol chloroform extraction) gave the best yield, enabling visualization of ethidium bromide-stained PCR product from a DNA dilution corresponding to 0.1 mm2 of tissue containing of the order of 10(3) nuclear profiles. Proteinase K digestion with detergents followed by phenol-chloroform extraction was no more effective than simple boiling. Although the success of PCR from preserved tissue will vary with the fixative and size of the amplified fragment, DNA extracted with this optimized method can be used for identification of viruses, loss of heterozygosity, and immunoglobulin gene rearrangements in paraffin-embedded tissue without radioisotopes.

Wind turbine extraction from high spatial resolution remote sensing images based on saliency detection

NASA Astrophysics Data System (ADS)

Chen, Jingbo; Yue, Anzhi; Wang, Chengyi; Huang, Qingqing; Chen, Jiansheng; Meng, Yu; He, Dongxu

2018-01-01

The wind turbine is a device that converts the wind's kinetic energy into electrical power. Accurate and automatic extraction of wind turbine is instructive for government departments to plan wind power plant projects. A hybrid and practical framework based on saliency detection for wind turbine extraction, using Google Earth image at spatial resolution of 1 m, is proposed. It can be viewed as a two-phase procedure: coarsely detection and fine extraction. In the first stage, we introduced a frequency-tuned saliency detection approach for initially detecting the area of interest of the wind turbines. This method exploited features of color and luminance, was simple to implement, and was computationally efficient. Taking into account the complexity of remote sensing images, in the second stage, we proposed a fast method for fine-tuning results in frequency domain and then extracted wind turbines from these salient objects by removing the irrelevant salient areas according to the special properties of the wind turbines. Experiments demonstrated that our approach consistently obtains higher precision and better recall rates. Our method was also compared with other techniques from the literature and proves that it is more applicable and robust.

Present state and perspective of downstream processing of biologically produced 1,3-propanediol and 2,3-butanediol.

PubMed

Xiu, Zhi-Long; Zeng, An-Ping

2008-04-01

1,3-Propanediol and 2,3-butanediol are two promising chemicals which have a wide range of applications and can be biologically produced. The separation of these diols from fermentation broth makes more than 50% of the total costs in their microbial production. This review summarizes the present state of methods studied for the recovery and purification of biologically produced diols, with particular emphasis on 1,3-propoanediol. Previous studies on the separation of 1,3-propanediol primarily include evaporation, distillation, membrane filtration, pervaporation, ion exchange chromatography, liquid-liquid extraction, and reactive extraction. Main methods for the recovery of 2,3-butanediol include steam stripping, pervaporation, and solvent extraction. No single method has proved to be simple and efficient, and improvements are especially needed with regard to yield, purity, and energy consumption. Perspectives for an improved downstream processing of biologically produced diols, especially 1,3-propanediol are discussed based on our own experience and recent work. It is argued that separation technologies such as aqueous two-phase extraction with short chain alcohols, pervaporation, reverse osmosis, and in situ extractive or pervaporative fermentations deserve more attention in the future.

Detection of Organophosphorus Pesticides in Wheat by Ionic Liquid-Based Dispersive Liquid-Liquid Microextraction Combined with HPLC

PubMed Central

Quan, Ji; Hu, Zeshu

2018-01-01

Food safety issues closely related to human health have always received widespread attention from the world society. As a basic food source, wheat is the fundamental support of human survival; therefore, the detection of pesticide residues in wheat is very necessary. In this work, the ultrasonic-assisted ionic liquid-dispersive liquid-liquid microextraction (DLLME) method was firstly proposed, and the extraction and analysis of three organophosphorus pesticides were carried out by combining high-performance liquid chromatography (HPLC). The extraction efficiencies of three ionic liquids with bis(trifluoromethylsulfonyl)imide (Tf2N) anion were compared by extracting organophosphorus in wheat samples. It was found that the use of 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([OMIM][Tf2N]) had both high enrichment efficiency and appropriate extraction recovery. Finally, the method was used for the determination of three wheat samples, and the recoveries of them were 74.8–112.5%, 71.8–104.5%, and 83.8–115.5%, respectively. The results show that the method proposed is simple, fast, and efficient, which can be applied to the extraction of organic matters in wheat samples. PMID:29854562

Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

NASA Astrophysics Data System (ADS)

Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

2016-09-01

The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

A novel fatty-acid-based in-tube dispersive liquid-liquid microextraction technique for the rapid determination of nonylphenol and 4-tert-octylphenol in aqueous samples using high-performance liquid chromatography-ultraviolet detection.

PubMed

Shih, Hou-Kuang; Shu, Ting-Yun; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2015-01-07

In this study, a novel fatty-acid-based in-tube dispersive liquid-liquid microextraction (FA-IT-DLLME) technique is proposed for the first time and is developed as a simple, rapid and eco-friendly sample extraction method for the determination of alkylphenols in aqueous samples using high-performance liquid chromatography-ultraviolet detection (HPLC-UV). In this extraction method, medium-chain saturated fatty acids were investigated as a pH-dependent phase because they acted as either anionic surfactants or neutral extraction solvents based on the acid-base reaction caused solely by the adjustment of the pH of the solution. A specially designed home-made glass extraction tube with a built-in scaled capillary tube was utilized as the phase-separation device for the FA-IT-DLLME to collect and measure the separated extractant phase for analysis. Nonylphenol (NP) and 4-tert-octylphenol (4-tOP) were chosen as model analytes. The parameters influencing the FA-IT-DLLME were thoroughly investigated and optimized. Under the optimal conditions, the detector responses of NP and 4-tOP were linear in the concentration ranges of 5-4000 μg L(-1), with correlation coefficients of 0.9990 and 0.9996 for NP and 4-tOP, respectively. The limits of detection based on a signal-to-noise ratio of 3 were 0.7 and 0.5 μg L(-1), and the enrichment factors were 195 and 143 for NP and 4-tOP, respectively. The applicability of the developed method was demonstrated for the analysis of alkylphenols in environmental wastewater samples, and the recoveries ranged from 92.9 to 107.1%. The extraction process required less than 4 min and utilized only acids, alkalis, and fatty acids to achieve the extraction. The results demonstrated that the presented FA-IT-DLLME approach is highly cost-effective, simple, rapid and environmentally friendly in its sample preparation. Copyright © 2014 Elsevier B.V. All rights reserved.

Efficient isolation method for high-quality genomic DNA from cicada exuviae.

PubMed

Nguyen, Hoa Quynh; Kim, Ye Inn; Borzée, Amaël; Jang, Yikweon

2017-10-01

In recent years, animal ethics issues have led researchers to explore nondestructive methods to access materials for genetic studies. Cicada exuviae are among those materials because they are cast skins that individuals left after molt and are easily collected. In this study, we aim to identify the most efficient extraction method to obtain high quantity and quality of DNA from cicada exuviae. We compared relative DNA yield and purity of six extraction protocols, including both manual protocols and available commercial kits, extracting from four different exoskeleton parts. Furthermore, amplification and sequencing of genomic DNA were evaluated in terms of availability of sequencing sequence at the expected genomic size. Both the choice of protocol and exuvia part significantly affected DNA yield and purity. Only samples that were extracted using the PowerSoil DNA Isolation kit generated gel bands of expected size as well as successful sequencing results. The failed attempts to extract DNA using other protocols could be partially explained by a low DNA yield from cicada exuviae and partly by contamination with humic acids that exist in the soil where cicada nymphs reside before emergence, as shown by spectroscopic measurements. Genomic DNA extracted from cicada exuviae could provide valuable information for species identification, allowing the investigation of genetic diversity across consecutive broods, or spatiotemporal variation among various populations. Consequently, we hope to provide a simple method to acquire pure genomic DNA applicable for multiple research purposes.

Determination of organophosphorus pesticides and their major degradation product residues in food samples by HPLC-UV.

PubMed

Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui

2016-10-01

A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.

Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection.

PubMed

Núñez, L; Turiel, E; Tadeo, J L

2007-04-06

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C(18) solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 microg/g). Under optimum conditions, 2g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 degrees C in two consecutive steps of 15 min using a mixture of H(2)O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C(18) cartridges, and analytes were eluted with 3 x 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 microl H(2)O/AcN (50/50), and passed though a 0.45 microm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.

A rapid method for the extraction and analysis of carotenoids and other hydrophobic substances suitable for systems biology studies with photosynthetic bacteria.

PubMed

Bóna-Lovász, Judit; Bóna, Aron; Ederer, Michael; Sawodny, Oliver; Ghosh, Robin

2013-10-11

A simple, rapid, and inexpensive extraction method for carotenoids and other non-polar compounds present in phototrophic bacteria has been developed. The method, which has been extensively tested on the phototrophic purple non-sulphur bacterium Rhodospirillum rubrum, is suitable for extracting large numbers of samples, which is common in systems biology studies, and yields material suitable for subsequent analysis using HPLC and mass spectroscopy. The procedure is particularly suitable for carotenoids and other terpenoids, including quinones, bacteriochlorophyll a and bacteriopheophytin a, and is also useful for the analysis of polar phospholipids. The extraction procedure requires only a single step extraction with a hexane/methanol/water mixture, followed by HPLC using a Spherisorb C18 column, with a mobile phase consisting of acetone-water and a non-linear gradient of 50%-100% acetone. The method was employed for examining the carotenoid composition observed during microaerophilic growth of R. rubrum strains, and was able to determine 18 carotenoids, 4 isoprenoid-quinones, bacteriochlorophyll a and bacteriopheophytin a as well as four different phosphatidylglycerol species of different acyl chain compositions. The analytical procedure was used to examine the dynamics of carotenoid biosynthesis in the major and minor pathways operating simultaneously in a carotenoid biosynthesis mutant of R. rubrum.

New method for the measurement of osmium isotopes applied to a New Zealand Cretaceous/Tertiary boundary shale

USGS Publications Warehouse

Lichte, F.E.; Wilson, S.M.; Brooks, R.R.; Reeves, R.D.; Holzbecher, J.; Ryan, D.E.

1986-01-01

The determination of osmium content and isotopic abundances in geological materials has received increasing attention in recent years following the proposal of Alvarez et al.1 that mass extinctions at the end of the Cretaceous period were caused by the impact of a large (???10km) meteorite which left anomalously high iridium levels as a geochemical signature in the boundary shales. Here we report a new and simple method for measuring osmium in geological materials, involving fusion of the sample with sodium peroxide, distillation of the osmium as the tetroxide using perchloric acid, extraction into chloroform, and absorption of the chloroform extract onto graphite powder before instrumental neutron activation analysis. In a variant of this technique, the chloroform extract is back-extracted into an aqueous phase and the osmium isotopes are determined by plasma-source mass spectrometry (ICPMS). We have used this method on the Woodside Creek (New Zealand) Cretaceous/Tertiary boundary clay and have obtained the first osmium content (6g ng g-1) for this material. The 187Os/186Os ratio is 1.12??0.16, showing a typical non-crustal signature. This combined distillation-extraction- ICPMS method will prove to be useful for measuring osmium isotopes in other geological materials. ?? 1986 Nature Publishing Group.

Green synthesis of silver nanoparticles mediated by Pulicaria glutinosa extract

PubMed Central

Khan, Mujeeb; Khan, Merajuddin; Adil, Syed Farooq; Tahir, Muhammad Nawaz; Tremel, Wolfgang; Alkhathlan, Hamad Z; Al-Warthan, Abdulrahman; Siddiqui, Mohammed Rafiq H

2013-01-01

The green synthesis of metallic nanoparticles (NPs) has attracted tremendous attention in recent years because these protocols are low cost and more environmentally friendly than standard methods of synthesis. In this article, we report a simple and eco-friendly method for the synthesis of silver NPs using an aqueous solution of Pulicaria glutinosa plant extract as a bioreductant. The as-prepared silver NPs were characterized using ultraviolet–visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier-transform infrared spectroscopy. Moreover, the effects of the concentration of the reductant (plant extract) and precursor solution (silver nitrate), the temperature on the morphology, and the kinetics of reaction were investigated. The results indicate that the size of the silver NPs varied as the plant extract concentration increased. The as-synthesized silver NPs were phase pure and well crystalline with a face-centered cubic structure. Further, Fourier-transform infrared spectroscopy analysis confirmed that the plant extract not only acted as a bioreductant but also functionalized the NPs’ surfaces to act as a capping ligand to stabilize them in the solvent. The developed eco-friendly method for the synthesis of NPs could prove a better substitute for the physical and chemical methods currently used to prepare metallic NPs commonly used in cosmetics, foods, and medicines. PMID:23620666

Qualitative and quantitative assessment of single fingerprints in forensic DNA analysis.

PubMed

Ostojic, Lana; Klempner, Stacey A; Patel, Rosni A; Mitchell, Adele A; Axler-DiPerte, Grace L; Wurmbach, Elisa

2014-11-01

Fingerprints and touched items are important sources of DNA for STR profiling, since this evidence can be recovered in a wide variety of criminal offenses. However, there are some fundamental difficulties in working with these samples, including variability in quantity and quality of extracted DNA. In this study, we collected and analyzed over 700 fingerprints. We compared a commercially available extraction protocol (Zygem) to two methods developed in our laboratory, a simple one-tube protocol and a high sensitivity protocol (HighSens) that includes additional steps to concentrate and purify the DNA. The amplification protocols tested were AmpFLSTR® Identifiler® using either 28 or 31 amplification cycles, and Identifiler® Plus using 32 amplification cycles. We found that the HighSens and Zygem extraction methods were significantly better in their DNA yields than the one-tube method. Identifiler® Plus increased the quality of the STR profiles for the one-tube extraction significantly. However, this effect could not be verified for the other extraction methods. Furthermore, microscopic analysis of single fingerprints revealed that some individuals tended to shed more material than others onto glass slides. However, a dense deposition of skin flakes did not strongly correlate with a high quality STR profile. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid and simple method by combining FTA™ card DNA extraction with two set multiplex PCR for simultaneous detection of non-O157 Shiga toxin-producing Escherichia coli strains and virulence genes in food samples.

PubMed

Kim, S A; Park, S H; Lee, S I; Ricke, S C

2017-12-01

The aim of this research was to optimize two multiplex polymerase chain reaction (PCR) assays that could simultaneously detect six non-O157 Shiga toxin-producing Escherichia coli (STEC) as well as the three virulence genes. We also investigated the potential of combining the FTA™ card-based DNA extraction with the multiplex PCR assays. Two multiplex PCR assays were optimized using six primer pairs for each non-O157 STEC serogroup and three primer pairs for virulence genes respectively. Each STEC strain specific primer pair only amplified 155, 238, 321, 438, 587 and 750 bp product for O26, O45, O103, O111, O121 and O145 respectively. Three virulence genes were successfully multiplexed: 375 bp for eae, 655 bp for stx1 and 477 bp for stx2. When two multiplex PCR assays were validated with ground beef samples, distinctive bands were also successfully produced. Since the two multiplex PCR examined here can be conducted under the same PCR conditions, the six non-O157 STEC and their virulence genes could be concurrently detected with one run on the thermocycler. In addition, all bands clearly appeared to be amplified by FTA card DNA extraction in the multiplex PCR assay from the ground beef sample, suggesting that an FTA card could be a viable sampling approach for rapid and simple DNA extraction to reduce time and labour and therefore may have practical use for the food industry. Two multiplex polymerase chain reaction (PCR) assays were optimized for discrimination of six non-O157 Shiga toxin-producing Escherichia coli (STEC) and identification of their major virulence genes within a single reaction, simultaneously. This study also determined the successful ability of the FTA™ card as an alternative to commercial DNA extraction method for conducting multiplex STEC PCR assays. The FTA™ card combined with multiplex PCR holds promise for the food industry by offering a simple and rapid DNA sample method for reducing time, cost and labour for detection of STEC in food and environmental samples. © 2017 The Society for Applied Microbiology.

Extraction and quantitative analysis of iodine in solid and solution matrixes.

PubMed

Brown, Christopher F; Geiszler, Keith N; Vickerman, Tanya S

2005-11-01

129I is a contaminant of interest in the vadose zone and groundwater at numerous federal and privately owned facilities. Several techniques have been utilized to extract iodine from solid matrixes; however, all of them rely on two fundamental approaches: liquid extraction or chemical/heat-facilitated volatilization. While these methods are typically chosen for their ease of implementation, they do not totally dissolve the solid. We defined a method that produces complete solid dissolution and conducted laboratory tests to assess its efficacy to extract iodine from solid matrixes. Testing consisted of potassium nitrate/potassium hydroxide fusion of the sample, followed by sample dissolution in a mixture of sulfuric acid and sodium bisulfite. The fusion extraction method resulted in complete sample dissolution of all solid matrixes tested. Quantitative analysis of 127I and 129I via inductively coupled plasma mass spectrometry showed better than +/-10% accuracy for certified reference standards, with the linear operating range extending more than 3 orders of magnitude (0.005-5 microg/L). Extraction and analysis of four replicates of standard reference material containing 5 microg/g 127I resulted in an average recovery of 98% with a relative deviation of 6%. This simple and cost-effective technique can be applied to solid samples of varying matrixes with little or no adaptation.

Application of ionic liquids in vacuum microwave-assisted extraction followed by macroporous resin isolation of three flavonoids rutin, hyperoside and hesperidin from Sorbus tianschanica leaves.

PubMed

Gu, Huiyan; Chen, Fengli; Zhang, Qiang; Zang, Jing

2016-03-01

Rutin, hyperoside and hesperidin were effectively extracted from Sorbus tianschanica leaves by an ionic liquid vacuum microwave-assisted method. A series of ionic liquids with various anions and alkyl chain length of the cations were studied and the extraction was performed in [C6mim][BF4] aqueous solution. After optimization by a factorial design and response surface methodology, total extraction yield of 2.37mg/g with an error of 0.12mg/g (0.71±0.04mg/g, 1.18±0.06mg/g and 0.48±0.02 for rutin, hyperoside and hesperidin, respectively) was achieved under -0.08MPa for vacuum, 19min and 420W for microwave irradiation time and power, and 15mL/g for liquid-solid ratio. The proposed method here is more efficient and needs a shorter extraction time for rutin, hyperoside and hesperidin from S. tianschanica leaves than reference extraction techniques. In stability studies performed with standard rutin, hyperoside and hesperidin, the target analytes were stable under the optimum conditions. The proposed method had a high reproducibility and precision. In addition, separation of rutin, hyperoside and hesperidin from [C6mim][BF4] extraction solution was completed effectively by AB-8 macroporous resin adsorption and desorption process. Ionic liquid vacuum microwave-assisted extraction is a simple, rapid and efficient sample extraction technique. Copyright © 2016 Elsevier B.V. All rights reserved.

Sensitive method for the quantitation of droloxifene in plasma and serum by high-performance liquid chromatography employing fluorimetric detection.

PubMed

Tess, D A; Cole, R O; Toler, S M

1995-12-15

A simple and highly sensitive reversed-phase fluorimetric HPLC method for the quantitation of droloxifene from rat, monkey, and human plasma as well as human serum is described. This assay employs solid-phase extraction and has a dynamic range of 25 to 10,000 pg/ml. Sample extraction (efficiencies > 86%) was accomplished using a benzenesulfonic acid (SCX) column with water and methanol rinses. Droloxifene and internal standard were eluted with 1 ml of 3.5% (v/v) ammonium hydroxide (30%) in methanol. Samples were quantitated using post-column UV-photochemical cyclization coupled with fluorimetric detection with excitation and emission wavelengths of 260 nm and 375 nm, respectively. Relative ease of sample extraction and short run times allow for the analysis of approximately 100 samples per day.

Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

PubMed Central

Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

2014-01-01

An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

Ligandless dispersive liquid--liquid microextraction of iron in biological and foodstuff samples and its determination by Electrothermal atomic absorption spectrometry.

PubMed

Madadizadeh, Mohadeseh; Taher, Mohammad Ali; Ashkenani, Hamid

2013-01-01

A new, simple, and efficient method comprising ligandless dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry is reported for the preconcentration and determination of ultratrace amounts of Fe(III). Carbon tetrachloride and acetone were used as the extraction and disperser solvents, respectively. Some effective parameters of the microextraction such as choice of extraction and disperser solvents, their volume, extraction time and temperature, salt and surfactant effect, and pH were optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.02 to 0.46 microg/L of Fe(III), with LOD and LOQ of 5.2 and 17.4 ng/L, respectively. The RSD for seven replicated determinations of Fe(IIl) ion at 0.1 microg/L concentration level was 5.2%. Operational simplicity, rapidity, low cost, good repeatability, and low consumption of extraction solvent are the main advantages of the proposed method. The method was successfully applied to the determination of iron in biological, food, and certified reference samples.

Molecularly imprinted solid-phase extraction for the determination of ten macrolide drugs residues in animal muscles by liquid chromatography-tandem mass spectrometry.

PubMed

Song, Xuqin; Zhou, Tong; Liu, Qingying; Zhang, Meiyu; Meng, Chenying; Li, Jiufeng; He, Limin

2016-10-01

A simple and sensitive method based on molecularly imprinted solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry was developed for the determination of the residues of ten macrolide drugs in swine, cattle and chicken muscles samples. The molecularly imprinted polymers (MIPs) were synthesized using tylosin as a template and methacrylic acid as a functional monomer. Samples were extracted with sodium borate buffer solution and ethyl acetate, and purified by the MIP cartridge. The results showed that the cartridge exhibited good recognition performance for macrolides, and better purification effect than the traditional solid-phase extraction cartridges. Recoveries of analytes at three spiking levels 1, 5 and 20μgkg(-1) ranged from 60.7% to 100.3% with the relative standard deviations less than 14%. The limits of detection of the method were between 0.1 and 0.4μgkg(-1). The method is useful for the routine monitoring of the residues of macrolide drugs in animal muscles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Evaluation of a method for the simultaneous quantification of N-nitrosamines in water samples based on stir bar sorptive extraction combined with high-performance liquid chromatography and diode array detection.

PubMed

Talebpour, Zahra; Rostami, Simindokht; Rezadoost, Hassan

2015-05-01

A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high-performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95-1000 ng/mL (r = 0.9995), 0.26-1000 ng/mL (r = 0.9988) and both 0.32-100 ng/mL (r = 0.9999) and 100-1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra- and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Network structure of multivariate time series.

PubMed

Lacasa, Lucas; Nicosia, Vincenzo; Latora, Vito

2015-10-21

Our understanding of a variety of phenomena in physics, biology and economics crucially depends on the analysis of multivariate time series. While a wide range tools and techniques for time series analysis already exist, the increasing availability of massive data structures calls for new approaches for multidimensional signal processing. We present here a non-parametric method to analyse multivariate time series, based on the mapping of a multidimensional time series into a multilayer network, which allows to extract information on a high dimensional dynamical system through the analysis of the structure of the associated multiplex network. The method is simple to implement, general, scalable, does not require ad hoc phase space partitioning, and is thus suitable for the analysis of large, heterogeneous and non-stationary time series. We show that simple structural descriptors of the associated multiplex networks allow to extract and quantify nontrivial properties of coupled chaotic maps, including the transition between different dynamical phases and the onset of various types of synchronization. As a concrete example we then study financial time series, showing that a multiplex network analysis can efficiently discriminate crises from periods of financial stability, where standard methods based on time-series symbolization often fail.

Determination of flavonoids from Orthosiphon stamineus in plasma using a simple HPLC method with ultraviolet detection.

PubMed

Loon, Yit Hong; Wong, Jia Woei; Yap, Siew Ping; Yuen, Kah Hay

2005-02-25

A simple liquid chromatographic method was developed for the simultaneous determination of flavonoids from Orthosiphon stamineus Benth, namely sinensitin, eupatorin and 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, in plasma. Prior to analysis, the flavonoids and the internal standard (naproxen) were extracted from plasma samples using a 1:1 mixture of ethyl acetate and chloroform. The detection and quantification limits for the three flavonoids were similar being 3 and 5 ng/ml, respectively. The within-day and between-day accuracy values, expressed as percentage of true values, for the three flavonoids were between 95 and 107%, while the corresponding precision, expressed as coefficients of variation, for the three flavonoids were less than 14%. In addition, the mean recovery values of the extraction procedure for all the flavonoids were between 92 and 114%. The calibration curves were linear over a concentration range of 5-4000 ng/ml. The present method was applied to analyse plasma samples obtained from a pilot study using rats in which the mean absolute oral bioavailability values for sinensitin, eupatorin and 3'-hydroxy-5,6,7,4'-tetramethoxyflavone was 9.4, 1.0 and 1.5%, respectively.

Dynamic ultrasonic nebulisation extraction coupled with headspace ionic liquid-based single-drop microextraction for the analysis of the essential oil in Forsythia suspensa.

PubMed

Yang, Jinjuan; Wei, Hongmin; Teng, Xiane; Zhang, Hanqi; Shi, Yuhua

2014-01-01

Ionic liquids have attracted much attention as an extraction solvent instead of traditional organic solvent in single-drop microextraction. However, non-volatile ionic liquids are difficult to couple with gas chromatography. Thus, the following injection system for the determination of organic compounds is described. To establish an environmentally friendly, simple, and effective extraction method for preparation and analysis of the essential oil from aromatic plants. The dynamic ultrasonic nebulisation extraction was coupled with headspace ionic liquid-based single-drop microextraction(UNE-HS/IL/SDME)for the extraction of essential oils from Forsythia suspense fruits. After 13 min of extraction for 50 mg sample, the extracts in ionic liquid were evaporated rapidly in the gas chromatography injector through a thermal desorption unit (5 s). The traditional extraction method was carried out for comparative study. The optimum conditions were: 3 μL of 1-methyl-3-octylimidazolium hexafluorophosphate was selected as the extraction solvent, the sample amount was 50 mg, the flow rate of purging gas was 200 mL/min, the extraction time was 13 min, the injection volume was 2 μL, and the thermal desorption temperature and time were 240 °C and 5 s respectively. Comparing with hydrodistillation (HD), the proposed method was environment friendly and efficient. The proposed method is environmentally friendly, time saving, with high efficiency and low consumption. It would extend the application range of the HS/SDME and would be useful especially for aromatic plants analysis. Copyright © 2013 John Wiley & Sons, Ltd.

Evaluation of the application of ERTS-1 data to the regional land use planning process. [Northeast Wisconsin

NASA Technical Reports Server (NTRS)

Clapp, J. L. (Principal Investigator); Green, T., III; Hanson, G. F.; Kiefer, R. W.; Niemann, B. J., Jr.

1974-01-01

The author has identified the following significant results. Employing simple and economical extraction methods, ERTS can provide valuable data to the planners at the state or regional level with a frequency never before possible. Interactive computer methods of working directly with ERTS digital information show much promise for providing land use information at a more specific level, since the data format production rate of ERTS justifies improved methods of analysis.

Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

PubMed

Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

2014-12-01

Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. Copyright © 2014 Elsevier B.V. All rights reserved.

Shape information from glucose curves: functional data analysis compared with traditional summary measures.

PubMed

Frøslie, Kathrine Frey; Røislien, Jo; Qvigstad, Elisabeth; Godang, Kristin; Bollerslev, Jens; Voldner, Nanna; Henriksen, Tore; Veierød, Marit B

2013-01-17

Plasma glucose levels are important measures in medical care and research, and are often obtained from oral glucose tolerance tests (OGTT) with repeated measurements over 2-3  hours. It is common practice to use simple summary measures of OGTT curves. However, different OGTT curves can yield similar summary measures, and information of physiological or clinical interest may be lost. Our mean aim was to extract information inherent in the shape of OGTT glucose curves, compare it with the information from simple summary measures, and explore the clinical usefulness of such information. OGTTs with five glucose measurements over two hours were recorded for 974 healthy pregnant women in their first trimester. For each woman, the five measurements were transformed into smooth OGTT glucose curves by functional data analysis (FDA), a collection of statistical methods developed specifically to analyse curve data. The essential modes of temporal variation between OGTT glucose curves were extracted by functional principal component analysis. The resultant functional principal component (FPC) scores were compared with commonly used simple summary measures: fasting and two-hour (2-h) values, area under the curve (AUC) and simple shape index (2-h minus 90-min values, or 90-min minus 60-min values). Clinical usefulness of FDA was explored by regression analyses of glucose tolerance later in pregnancy. Over 99% of the variation between individually fitted curves was expressed in the first three FPCs, interpreted physiologically as "general level" (FPC1), "time to peak" (FPC2) and "oscillations" (FPC3). FPC1 scores correlated strongly with AUC (r=0.999), but less with the other simple summary measures (-0.42≤r≤0.79). FPC2 scores gave shape information not captured by simple summary measures (-0.12≤r≤0.40). FPC2 scores, but not FPC1 nor the simple summary measures, discriminated between women who did and did not develop gestational diabetes later in pregnancy. FDA of OGTT glucose curves in early pregnancy extracted shape information that was not identified by commonly used simple summary measures. This information discriminated between women with and without gestational diabetes later in pregnancy.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An extension of the Coconut Cream Agar method to screen Penicillium citrinum isolates for citrinin production.

PubMed

Mohamed, S; Flint, S; Palmer, J; Fletcher, G C; Pitt, J I

2013-09-01

A simple and rapid screening method was developed for the detection of citrinin in fungal cultures using Coconut Cream Agar (CCA) described previously for detecting aflatoxin and ochratoxin A. Fifteen isolates of Penicillium citrinum were inoculated onto CCA and incubated at 25 and 30°C for 10 days. All isolates produced a distinct yellow green fluorescence on CCA when the reverse side of the agar plates were viewed under long wavelength UV light. Detection was optimal at 25°C after four to 5 days of incubation. Isolates positive by the CCA method also tested positive for citrinin production by the TLC agar plug method after growth on CCA, Czapek yeast extract agar and yeast extract sucrose agar. Control cultures were negative by both methods, indicating that the CCA Petri dish method was suitable for screening cultures for citrinin production. © 2013 The Society for Applied Microbiology.

Electrogeochemical sampling with NEOCHIM - results of tests over buried gold deposits

USGS Publications Warehouse

Leinz, R.W.; Hoover, D.B.; Fey, D.L.; Smith, D.B.; Patterson, T.

1998-01-01

Electrogeochemical extraction methods are based on the migration of ions in an electric field. Ions present in soil moisture are transported by an applied current into fluids contained in special electrodes placed on the soil. The fluids are then collected and analyzed. Extractions are governed by Faraday's and Ohm's laws and are modeled by the operation of a simple Hittord transference apparatus. Calculations show that the volume of soil sampled in an ideal electrogeochemical extraction can be orders of magnitude greater than the volumes used in more popular geochemical extraction methods, although this has not been verified experimentally. CHIM is a method of in-situ electrogeochemical extraction that was developed in the former Soviet Union and has been tested and applied internationally to exploration for buried mineral deposits. Tests carried out at the US Geological Survey (USGS) indicated that there were problems inherent in the use of CHIM technology. The cause of the problems was determined to be the diffusion of acid from the conventional electrode into the soil. The NEOCHIM electrode incorporates two compartments and a salt bridge in a design that inhibits diffusion of acid and enables the collection of anions or cations. Tests over a gold-enriched vein in Colorado and over buried, Carlin-type, disseminated gold deposits in northern Nevada show that there are similarities and differences between NEOCHIM results and those by partial extractions of soils which include simple extractions with water, dilute acids and solutions of salts used as collector fluids in the electrodes. Results of both differ from the results obtained by total chemical digestion. The results indicate that NEOCHIM responds to mineralized faults associated with disseminated gold deposits whereas partial and total chemical extraction methods do not. This suggests that faults are favored channels for the upward migration of metals and that NEOCHIM may be more effective in exploration for the deposits. It defines anomalies that are often narrow and intense, an observation previously made by CHIM researchers. The field tests show that NEOCHIM is less affected by surface contamination. A test over the Mike disseminated gold deposit indicates that the method may not be effective for locating deposits with impermeable cover. Faradaic extraction efficiencies of 20-30%, or more, are frequently achieved with NEOCHIM and the method generally shows good reproducibility, especially in extraction of major cations. However, ions of other metals that are useful in exploration, including Au and As, may be collected in low and temporally variable concentrations. The reason for this variability is unclear and requires further investigation.CHIM is a method of in-situ electrogeochemical extraction developed for the exploration of buried mineral deposits. However, electrode problems like diffusion of acid into the soil were encountered during the use of CHIM. The NEOCHIM electrode was developed to inhibit the diffusion of acid and enable collection of anions or cations. Tests over buried gold deposits showed that NEOCHIM responds to mineralized faults associated with disseminated gold deposits whereas partial and total chemical extraction methods do not. This suggests that faults are favored channels for the upward migration of metals and NEOCHIM may be effective in exploration for the deposits. But ions of metals may be collected in low and variable concentration.

Simple and Fast Sample Preparation Followed by Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS) for the Analysis of 2- and 4-Methylimidazole in Cola and Dark Beer.

PubMed

Choi, Sol Ji; Jung, Mun Yhung

2017-04-01

We have developed a simple and fast sample preparation technique in combination with a gas chromatography-tandem mass spectrometry (GC-MS/MS) for the quantification of 2-methylimidazole (2-MeI) and 4-methylimidazole (4-MeI) in colas and dark beers. Conventional sample preparation technique for GC-MS requires laborious and time-consuming steps consisting of sample concentration, pH adjustment, ion pair extraction, centrifugation, back-extraction, centrifugation, derivatization, and extraction. Our sample preparation technique consists of only 2 steps (in situ derivation and extraction) which requires less than 3 min. This method provided high linearity, low limit of detection and limit of quantification, high recovery, and high intra- and interday repeatability. It was found that internal standard method with diluted stable isotope (4-MeI-d 6 ) and 2-ethylimidazole (2-EI) could not correctly compensate the matrix effects. Thus, standard addition technique was used for the quantification of 2- and 4-MeI. The established method was successfully applied to colas and dark beers for the determination of 2-MeI and 4-MeI. The 4-MeI contents in colas and dark beers ranged from 8 to 319 μg/L and from trace to 417 μg/L, respectively. Small quantity (0 to 8 μg/L) of 2-MeI was found only in dark beers. The contents of 4-MeI (22 μg/L) in colas obtained from fast food restaurants were significantly lower than those (177 μg/L) in canned or bottled colas. © 2017 Institute of Food Technologists®.

Rapid investigation of α-glucosidase inhibitory activity of Phaleria macrocarpa extracts using FTIR-ATR based fingerprinting.

PubMed

Easmin, Sabina; Sarker, Md Zaidul Islam; Ghafoor, Kashif; Ferdosh, Sahena; Jaffri, Juliana; Ali, Md Eaqub; Mirhosseini, Hamed; Al-Juhaimi, Fahad Y; Perumal, Vikneswari; Khatib, Alfi

2017-04-01

Phaleria macrocarpa, known as "Mahkota Dewa", is a widely used medicinal plant in Malaysia. This study focused on the characterization of α-glucosidase inhibitory activity of P. macrocarpa extracts using Fourier transform infrared spectroscopy (FTIR)-based metabolomics. P. macrocarpa and its extracts contain thousands of compounds having synergistic effect. Generally, their variability exists, and there are many active components in meager amounts. Thus, the conventional measurement methods of a single component for the quality control are time consuming, laborious, expensive, and unreliable. It is of great interest to develop a rapid prediction method for herbal quality control to investigate the α-glucosidase inhibitory activity of P. macrocarpa by multicomponent analyses. In this study, a rapid and simple analytical method was developed using FTIR spectroscopy-based fingerprinting. A total of 36 extracts of different ethanol concentrations were prepared and tested on inhibitory potential and fingerprinted using FTIR spectroscopy, coupled with chemometrics of orthogonal partial least square (OPLS) at the 4000-400 cm -1 frequency region and resolution of 4 cm -1 . The OPLS model generated the highest regression coefficient with R 2 Y = 0.98 and Q 2 Y = 0.70, lowest root mean square error estimation = 17.17, and root mean square error of cross validation = 57.29. A five-component (1+4+0) predictive model was build up to correlate FTIR spectra with activity, and the responsible functional groups, such as -CH, -NH, -COOH, and -OH, were identified for the bioactivity. A successful multivariate model was constructed using FTIR-attenuated total reflection as a simple and rapid technique to predict the inhibitory activity. Copyright © 2016. Published by Elsevier B.V.

Optimized emission in nanorod arrays through quasi-aperiodic inverse design.

PubMed

Anderson, P Duke; Povinelli, Michelle L

2015-06-01

We investigate a new class of quasi-aperiodic nanorod structures for the enhancement of incoherent light emission. We identify one optimized structure using an inverse design algorithm and the finite-difference time-domain method. We carry out emission calculations on both the optimized structure as well as a simple periodic array. The optimized structure achieves nearly perfect light extraction while maintaining a high spontaneous emission rate. Overall, the optimized structure can achieve a 20%-42% increase in external quantum efficiency relative to a simple periodic design, depending on material quality.

Improved Proteomic Analysis Following Trichloroacetic Acid Extraction of Bacillus anthracis Spore Proteins

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

Kaiser, Brooke LD; Wunschel, David S.; Sydor, Michael A.

2015-08-07

Proteomic analysis of bacterial samples provides valuable information about cellular responses and functions under different environmental pressures. Proteomic analysis is dependent upon efficient extraction of proteins from bacterial samples without introducing bias toward extraction of particular protein classes. While no single method can recover 100% of the bacterial proteins, selected protocols can improve overall protein isolation, peptide recovery, or enrich for certain classes of proteins. The method presented here is technically simple and does not require specialized equipment such as a mechanical disrupter. Our data reveal that for particularly challenging samples, such as B. anthracis Sterne spores, trichloroacetic acid extractionmore » improved the number of proteins identified within a sample compared to bead beating (714 vs 660, respectively). Further, TCA extraction enriched for 103 known spore specific proteins whereas bead beating resulted in 49 unique proteins. Analysis of C. botulinum samples grown to 5 days, composed of vegetative biomass and spores, showed a similar trend with improved protein yields and identification using our method compared to bead beating. Interestingly, easily lysed samples, such as B. anthracis vegetative cells, were equally as effectively processed via TCA and bead beating, but TCA extraction remains the easiest and most cost effective option. As with all assays, supplemental methods such as implementation of an alternative preparation method may provide additional insight to the protein biology of the bacteria being studied.« less

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

PubMed

Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

2016-05-15

A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

A method for extracting high-quality total RNA from plant rich in polysaccharides and polyphenols using Dendrobium huoshanense

PubMed Central

Yu, Nianjun; Zhang, Wei; Xing, Lihua; Xie, Dongmei; Peng, Daiyin

2018-01-01

Acquiring high quality RNA is the basis of plant molecular biology research, plant genetics and other physiological investigations. At present, a large number of nucleotide isolation methods have been exploited or modified, such as commercial kits, CTAB, SDS methods and so on. Due to the nature of different plants, extraction methods vary. Moreover, efficiency of certain approach cannot be guaranteed due to composition of different plants and extracting high quality RNA from plants rich in polysaccharides and polyphenols are often difficult. The physical and chemical properties of polysaccharides which are similar to nucleic acids and other secondary metabolites will be coprecipitated with RNA irreversibly. Therefore, how to remove polysaccharides and other secondary metabolites during RNA extraction is the primary challenge. Dendrobium huoshanense is an Orchidaceae perennial herb that is rich in polysaccharides and other secondary metabolites. By using D. huoshanense as the subject, we improved the method originated from CHAN and made it suitable for plants containing high amount of polysaccharides and polyphenols. The extracted total RNA was clear and non-dispersive, with good integrity and no obvious contamination with DNA and other impurities. And it was also evaluated by gel electrophoresis, nucleic acid quantitative detector and PCR assessment. Thus, as a simple approach, it is suitable and efficient in RNA isolation for plants rich in polysaccharides and polyphenols. PMID:29715304

Polydimethylsiloxane rod extraction, a novel technique for the determination of organic micropollutants in water samples by thermal desorption-capillary gas chromatography-mass spectrometry.

PubMed

Montero, L; Popp, P; Paschke, A; Pawliszyn, J

2004-01-30

A novel, simple and inexpensive approach to absorptive extraction of organic compounds from environmental samples is presented. It consists of a polydimethylsiloxane rod used as an extraction media, enriched with analytes during shaking, then thermally desorbed and analyzed by GC-MS. Its performance was illustrated and evaluated for the enrichment of sub- to ng/l of selected chlorinated compounds (chlorobenzenes and polychlorinated biphenyls) in water samples. The new approach was compared to the stir bar sorptive extraction performance. A natural ground water sample from Bitterfeld, Germany, was also extracted using both methods, showing good agreement. The proposed approach presented good linearity, high sensitivity, good blank levels and recoveries comparable to stir bars, together with advantages such as simplicity, lower cost and higher feasibility.

Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

NASA Astrophysics Data System (ADS)

Yokochi, Reika

2016-09-01

Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters by use of solid-phase extraction, and its applications to brackish lake waters.

PubMed

Okumura, M; Tong, L; Fujinaga, K; Seike, Y

2001-05-01

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters has been developed for field analysis. This method is based on solid-phase extraction on a zirconium-loaded Sep-Pack Accell CM cartridge (Zr-SP) and is applicable to studies in which sampling is performed by use of a graduated syringe to prevent contamination and to ensure easy operation at sampling sites. The Zr-SP cartridge was prepared by passing 0.1 mol L(-1) zirconium solution through a Sep-Pak Accell CM cartridge, packed with cation exchange sorbent based on a silica matrix. The adsorption of phosphate and its desorption depend only on the pH of the solution. A water sample containing phosphate was adjusted to pH 2 and passed through the Zr-SP cartridge to collect it. The retained phosphate was quantitatively eluted with 0.5 mol L(-1) sodium hydroxide solution. The phosphate retained in the Zr-SP cartridge was stable for at least one month. The established preconcentration method was successfully applied to brackish lake waters to investigate seasonal changes in the distribution and behavior of phosphate in a brackish lake.

Multiscale moment-based technique for object matching and recognition

NASA Astrophysics Data System (ADS)

Thio, HweeLi; Chen, Liya; Teoh, Eam-Khwang

2000-03-01

A new method is proposed to extract features from an object for matching and recognition. The features proposed are a combination of local and global characteristics -- local characteristics from the 1-D signature function that is defined to each pixel on the object boundary, global characteristics from the moments that are generated from the signature function. The boundary of the object is first extracted, then the signature function is generated by computing the angle between two lines from every point on the boundary as a function of position along the boundary. This signature function is position, scale and rotation invariant (PSRI). The shape of the signature function is then described quantitatively by using moments. The moments of the signature function are the global characters of a local feature set. Using moments as the eventual features instead of the signature function reduces the time and complexity of an object matching application. Multiscale moments are implemented to produce several sets of moments that will generate more accurate matching. Basically multiscale technique is a coarse to fine procedure and makes the proposed method more robust to noise. This method is proposed to match and recognize objects under simple transformation, such as translation, scale changes, rotation and skewing. A simple logo indexing system is implemented to illustrate the performance of the proposed method.

Development and validation of an RP-HPLC method for the quantitation of odanacatib in rat and human plasma and its application to a pharmacokinetic study.

PubMed

Police, Anitha; Gurav, Sandip; Dhiman, Vinay; Zainuddin, Mohd; Bhamidipati, Ravi Kanth; Rajagopal, Sriram; Mullangi, Ramesh

2015-11-01

A simple, specific, sensitive and reproducible high-performance liquid chromatography (HPLC) assay method has been developed and validated for the estimation of odanacatib in rat and human plasma. The bioanalytical procedure involves extraction of odanacatib and itraconazole (internal standard, IS) from a 200 μL plasma aliquot with simple liquid-liquid extraction process. Chromatographic separation was achieved on a Symmetry Shield RP18 using an isocratic mobile phase at a flow rate of 0.7 mL/min. The UV detection wave length was 268 nm. Odanacatib and IS eluted at 5.5 and 8.6 min, respectively with a total run time of 10 min. Method validation was performed as per US Food and Drug Administration guidelines and the results met the acceptance criteria. The calibration curve was linear over a concentration range of 50.9-2037 ng/mL (r(2) = 0.994). The intra- and inter-day precisions were in the range of 2.06-5.11 and 5.84-13.1%, respectively, in rat plasma and 2.38-7.90 and 6.39-10.2%, respectively, in human plasma. The validated HPLC method was successfully applied to a pharmacokinetic study in rats. Copyright © 2015 John Wiley & Sons, Ltd.

Simple and fast method for iron determination in white and red wines using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry.

PubMed

Maciel, Juliana V; Soares, Bruno M; Mandlate, Jaime S; Picoloto, Rochele S; Bizzi, Cezar A; Flores, Erico M M; Duarte, Fabio A

2014-08-20

This work reports the development of a method for Fe extraction in white and red wines using dispersive liquid-liquid microextraction (DLLME) and determination by ultraviolet-visible spectrophotometry. For optimization of the DLLME method, the following parameters were evaluated: type and volume of dispersive (1300 μL of acetonitrile) and extraction (80 μL of C(2)Cl(4)) solvents, pH (3.0), concentration of ammonium pyrrolidinedithiocarbamate (APDC, 500 μL of 1% m/v APDC solution), NaCl concentration (not added), and extraction time. The calibration curve was performed using the analyte addition method, and the limit of detection and relative standard deviation were 0.2 mg L(-1) and below 7%, respectively. The accuracy was evaluated by comparison of results obtained after Fe determination by graphite furnace atomic absorption spectrometry, with agreement ranging from 94 to 105%. The proposed method was applied for Fe determination in white and red wines with concentrations ranging from 1.3 to 4.7 mg L(-1).

Possible Explanation of the Different Temporal Behaviors of Various Classes of Sunspot Groups

NASA Astrophysics Data System (ADS)

Gao, Peng-Xin; Li, Ke-Jun; Li, Fu-Yu

2017-09-01

In order to investigate the periodicity and long-term trends of various classes of sunspot groups (SGs), we separated SGs into two categories: simple SGs (A/U ≤ 4.5, where A represents the total corrected whole spot area of the group in millionths of the solar hemisphere (msh), and U represents the total corrected umbral area of the group in msh); and complex SGs (A/U > 6.2). Based on the revised version of the Greenwich Photoheliographic Results sunspot catalogue, we investigated the periodic behaviors and long-term trends of simple and complex SGs from 1875 to 1976 using the Hilbert-Huang Transform method, and we confirm that the temporal behaviors of simple and complex SGs are quite different. Our main findings are as follows. i) For simple and complex SGs, the values of the Schwabe cycle wax and wane, following the solar activity cycle. ii) There are significant phase differences (almost antiphase) between the periodicity of 53.50 ± 3.79 years extracted from yearly simple SG numbers and the periodicity of 56.21 ± 2.92 years extracted from yearly complex SG numbers. iii) The adaptive trends of yearly simple and complex SG numbers are also quite different: for simple SGs, the values of the adaptive trend gradually increase during the time period of 1875 - 1949, then they decrease gradually from 1949 to 1976, similar to the rise and the maximum phase of a sine curve; for complex SGs, the values of the adaptive trend first slowly increase and then quickly increase, similar to the minimum and rise phase of a sine curve.

Spectrophotometric total reducing sugars assay based on cupric reduction.

PubMed

Başkan, Kevser Sözgen; Tütem, Esma; Akyüz, Esin; Özen, Seda; Apak, Reşat

2016-01-15

As the concentration of reducing sugars (RS) is controlled by European legislation for certain specific food and beverages, a simple and sensitive spectrophotometric method for the determination of RS in various food products is proposed. The method is based on the reduction of Cu(II) to Cu(I) with reducing sugars in alkaline medium in the presence of 2,9-dimethyl-1,10-phenanthroline (neocuproine: Nc), followed by the formation of a colored Cu(I)-Nc charge-transfer complex. All simple sugars tested had the linear regression equations with almost equal slope values. The proposed method was successfully applied to fresh apple juice, commercial fruit juices, milk, honey and onion juice. Interference effect of phenolic compounds in plant samples was eliminated by a solid phase extraction (SPE) clean-up process. The method was proven to have higher sensitivity and precision than the widely used dinitrosalicylic acid (DNS) colorimetric method. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple, sensitive determination of ganciclovir in infant plasma by high-performance liquid chromatography with fluorescence detection.

PubMed

Yoshida, Terumitsu; Takahashi, Ryohei; Imai, Koichi; Uchida, Hiroshi; Arai, Yasutoshi; Oh-ishi, Tsutomu

2010-03-01

This study developed a simple and sensitive method using reversed-phase high-performance liquid chromatography (HPLC) for ganciclovir (GCV) plasma concentrations in cytomegalovirus infectious infants with hearing loss. The method involves a simple protein precipitation procedure that uses no solid-phase or liquid-liquid extraction. The HPLC separation was carried out on a Cadenza CD-C(18) column (3 microm, 4.6 mm x 150 mm) with phosphate buffer (pH 2.5, 25 mM) containing 1% methanol-acetonitrile mixture (4:3, v/v) as a mobile phase at a 0.7 mL/min flow rate. GCV was detected using a fluorescence detection (lambdaex/em: 265/380 nm). The quantification limit was 0.025 microg/mL for 100 microL of plasma sample at which good intra- and inter-assay coefficient of variation values (< 4.96%) and recoveries (94.9-96.5%) were established.

Unsteady hovering wake parameters identified from dynamic model tests, part 1

NASA Technical Reports Server (NTRS)

Hohenemser, K. H.; Crews, S. T.

1977-01-01

The development of a 4-bladed model rotor is reported that can be excited with a simple eccentric mechanism in progressing and regressing modes with either harmonic or transient inputs. Parameter identification methods were applied to the problem of extracting parameters for linear perturbation models, including rotor dynamic inflow effects, from the measured blade flapping responses to transient pitch stirring excitations. These perturbation models were then used to predict blade flapping response to other pitch stirring transient inputs, and rotor wake and blade flapping responses to harmonic inputs. The viability and utility of using parameter identification methods for extracting the perturbation models from transients are demonstrated through these combined analytical and experimental studies.

Novel approaches mediated by tailor-made green solvents for the extraction of phenolic compounds from agro-food industrial by-products.

PubMed

Fernández, María de Los Ángeles; Espino, Magdalena; Gomez, Federico J V; Silva, María Fernanda

2018-01-15

An environmentally friendly method for the phenolic compound extraction from agro-food industrial by-products was developed in order to contribute with their sustainable valorization. A Natural Deep Eutectic Solvent was chemometrically-designed for the first time and compared with traditional solvents in terms of analyte stabilization. The combination of lactic acid, glucose and 15% water (LGH-15) was selected as optimal. A high-efficiency ultrasound-assisted extraction mediated by LGH-15 prior to HPLC-DAD allows the determination of 14 phenols in onion, olive, tomato and pear industrial by-products. NADES synthesis as well as the extraction procedures were optimized by Response Surface Methodology. Thus, phenolic determination in these complex samples was achieved by a simple, non-expensive, eco-friendly and robust system. The application to different matrices demonstrated the versatility of the proposed method. NADES opens interesting perspectives for their potential use as vehicles of bioactive compounds as food additives or pharmaceuticals. Copyright © 2017 Elsevier Ltd. All rights reserved.

Improvement of the ESR detection of irradiated food containing cellulose employing a simple extraction method

NASA Astrophysics Data System (ADS)

Delincée, Henry; Soika, Christiane

2002-03-01

Fruit may be irradiated at rather low doses, below 1 kGy in combination treatments or for quarantine purposes. To improve the ESR detection sensitivity of irradiated fruit de Jesus et al. (Int. J. Food Sci. Technol. 34 (1999) 173.) proposed extracting the fruit pulp with 80% ethanol and measuring the residue with ESR using low power (0.25 mW) for detection of 'cellulosic' radicals. An improvement in ESR sensitivity using the extraction procedure could be confirmed in this paper for strawberries and papayas. In most cases, a radiation dose of 0.5 kGy could be detected in both fruits even after 2-3 weeks storage. In addition, some herbs and spices were also tested, but only for a few of them the ESR detection of the 'cellulosic' signal was improved by previous alcoholic extraction. As an alternative to ESR measurements, other detection methods like DNA Comet Assay and thermoluminescence were also tested.

Capillary-driven microfluidic paper-based analytical devices for lab on a chip screening of explosive residues in soil.

PubMed

Ueland, Maiken; Blanes, Lucas; Taudte, Regina V; Stuart, Barbara H; Cole, Nerida; Willis, Peter; Roux, Claude; Doble, Philip

2016-03-04

A novel microfluidic paper-based analytical device (μPAD) was designed to filter, extract, and pre-concentrate explosives from soil for direct analysis by a lab on a chip (LOC) device. The explosives were extracted via immersion of wax-printed μPADs directly into methanol soil suspensions for 10min, whereby dissolved explosives travelled upwards into the μPAD circular sampling reservoir. A chad was punched from the sampling reservoir and inserted into a LOC well containing the separation buffer for direct analysis, avoiding any further extraction step. Eight target explosives were separated and identified by fluorescence quenching. The minimum detectable amounts for all eight explosives were between 1.4 and 5.6ng with recoveries ranging from 53-82% from the paper chad, and 12-40% from soil. This method provides a robust and simple extraction method for rapid identification of explosives in complex soil samples. Copyright © 2016 Elsevier B.V. All rights reserved.

GC-MS determination of parabens, triclosan and methyl triclosan in water by in situ derivatisation and stir-bar sorptive extraction.

PubMed

Casas Ferreira, Ana María; Möder, Monika; Fernández Laespada, María Esther

2011-01-01

Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption-gas chromatography-mass spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature) were optimised using a Box-Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben (22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated wastewater.

Determination of bulk and interface density of states in metal oxide semiconductor thin-film transistors by using capacitance-voltage characteristics

NASA Astrophysics Data System (ADS)

Wei, Xixiong; Deng, Wanling; Fang, Jielin; Ma, Xiaoyu; Huang, Junkai

2017-10-01

A physical-based straightforward extraction technique for interface and bulk density of states in metal oxide semiconductor thin film transistors (TFTs) is proposed by using the capacitance-voltage (C-V) characteristics. The interface trap density distribution with energy has been extracted from the analysis of capacitance-voltage characteristics. Using the obtained interface state distribution, the bulk trap density has been determined. With this method, for the interface trap density, it is found that deep state density nearing the mid-gap is approximately constant and tail states density increases exponentially with energy; for the bulk trap density, it is a superposition of exponential deep states and exponential tail states. The validity of the extraction is verified by comparisons with the measured current-voltage (I-V) characteristics and the simulation results by the technology computer-aided design (TCAD) model. This extraction method uses non-numerical iteration which is simple, fast and accurate. Therefore, it is very useful for TFT device characterization.

Preparation and evaluation of a mixed-bed immunoaffinity column for selective purification of sixteen sulfonamides in pork muscle.

PubMed

Li, Yingguo; Chen, Yiqiang; Li, Zhengguo; Zhang, Lei; Li, Xianliang; Xi, Cunxian; Wang, Guomin; Wang, Xiong; Guo, Qi; Li, Na

2012-03-01

This paper describes the preparation of a novel mixed-bed immunoaffinity chromatography (IAC) column by coupling four monoclonal antibodies against different sulfonamides (SAs) to Sepharose 4B. The IAC column can be used to simultaneously extract and purify 16 SAs in pork muscle. The dynamic column capacities for all SAs in mixed standard solution were between 312 and 479 ng/mL gel. After simple extraction and IAC cleanup, the sample solution can be directly injected for liquid chromatography-ultraviolet analysis. The recoveries of SAs from spiked samples at levels of 25, 50 and 100 µg/kg ranged from 83.3 to 103.1% with variation coefficient less than 8.6%. The comparison of IAC with liquid-liquid extraction and solid phase extraction indicated that IAC has better purification effect and needs less organic solution than conventional methods, thus it would be an ideal method for selective purification of SAs in pork muscle.

Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

PubMed

Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Iron oxide functionalized graphene oxide as an efficient sorbent for dispersive micro-solid phase extraction of sulfadiazine followed by spectrophotometric and mode-mismatched thermal lens spectrometric determination.

PubMed

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

2016-01-15

A simple and rapid dispersive micro-solid phase extraction (DMSPE) combined with mode-mismatched thermal lens spectrometry as well as fiber optic linear array spectrophotometry was developed for the separation, extraction and determination of sulfadiazine. Graphene oxide was synthesized using the modified Hummers method and functionalized with iron oxide nanoparticles by means of a simple one step chemical coprecipitation method. The synthesized iron oxide functionalized graphene oxide was utilized as an efficient sorbent in DMSPE of sulfadiazine. The retained analyte was eluted by using 180µL of a 6:4 mixture of methanol/acetic acid solution and was spectrophotometrically determined based on the formation of an azo dye through coupling with thenoyltrifluoroacetone. Under the optimized conditions, with the application of spectrophotometry technique and with a sample volume of 100mL, the method exhibited a linear dynamic range of 3-80µg L(-1) with a detection limit of 0.82µg L(-1), an enrichment factor of 200 as well as the relative standard deviations of 2.6% and 4.3% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. Whereas, through the application of the thermal lens spectrometry and a sample volume of 10mL, the method exhibited a linear dynamic range of 1-800µg L(-1) with a detection limit of 0.34µg L(-1) and the relative standard deviations of 3.1% and 5.4% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. The method was successfully applied to the determination of sulfadiazine in milk, honey and water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous Preconcentration and Determination of Brilliant Blue and Sunset Yellow in Foodstuffs by Solid-Phase Extraction Combined UV-Vis Spectrophotometry.

PubMed

Bişgin, Abdullah Taner

2018-05-29

Background: Brilliant Blue and Sunset Yellow, two highly water-soluble synthetic food dyes, are the most popular food dyes used and consumed. Although they are not highly toxic, some health problems can be observed when excessive amounts of food products containing these dyes are consumed. Objectives: The aim of the study was to develop a simultaneous UV-Vis combined solid-phase extraction method, based on the adsorption onto Amberlite XAD-8 resin, for determination of Brilliant Blue and Sunset Yellow dyes. Methods: Sample solution was poured into the reservoir of the column and permitted to gravitationally pass through the column at 2 mL/min flow rate. Adsorbed dyes were eluted to 5 mL of final volume with 1 mol/L HNO₃ in ethanol solution by applying a 2 mL/min flow rate. Dye concentrations of the solution were determined at 483 and 630 nm for Sunset Yellow and Brilliant Blue, respectively. Results: The detection limits of the method for Brilliant Blue and Sunset Yellow were determined as 0.13 and 0.66 ng/mL, respectively. Preconcentration factor was 80. Brilliant Blue contents of real food samples were found to be between 11 and 240 μg/g. Sunset Yellow concentrations of foodstuffs were determined to be between 19 and 331 μg/g. Conclusions: Economical, effective, and simple simultaneous determination of Brilliant Blue and Sunset Yellow was achieved by using a solid-phase extraction combined UV-Vis spectrometry method. Highlights: The method is applicable and suitable for routine analysis in quality control laboratories without the need for expert personnel and high operational costs because the instrumentation is simple and inexpensive.

Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

PubMed

Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

2017-08-01

A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detection of Legume Protease Inhibitors by the Gel-X-ray Film Contact Print Technique

ERIC Educational Resources Information Center

Mulimani, Veerappa H.; Sudheendra, Kulkarni; Giri, Ashok P.

2002-01-01

Redgram (Cajanus cajan L.) extracts have been analyzed for the protease inhibitors using a new, sensitive, simple, and rapid method for detection of electrophoretically separated protease inhibitors. The detection involves equilibrating the gel successively in the protease assay buffer and protease solution, rinsing the gel in assay buffer, and…

Identification and Quantitation of Various Inositols and O-methylinositols Present in Plant Roots Using Gas Chromatograpghy/Mass Spectrometry

USDA-ARS?s Scientific Manuscript database

Many inositols and O-methylinositols serve important roles in medicine and plant biology. A simple method was developed for the identification of these compounds in plant roots by extracting with 80% ethanol, derivatizing with trimethylsilyl imidazole, and analyzing by gas chromatography/mass spect...

[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.

JMOSFET: A MOSFET parameter extractor with geometry-dependent terms

NASA Technical Reports Server (NTRS)

Buehler, M. G.; Moore, B. T.

1985-01-01

The parameters from metal-oxide-silicon field-effect transistors (MOSFETs) that are included on the Combined Release and Radiation Effects Satellite (CRRES) test chips need to be extracted to have a simple but comprehensive method that can be used in wafer acceptance, and to have a method that is sufficiently accurate that it can be used in integrated circuits. A set of MOSFET parameter extraction procedures that are directly linked to the MOSFET model equations and that facilitate the use of simple, direct curve-fitting techniques are developed. In addition, the major physical effects that affect MOSFET operation in the linear and saturation regions of operation for devices fabricated in 1.2 to 3.0 mm CMOS technology are included. The fitting procedures were designed to establish single values for such parameters as threshold voltage and transconductance and to provide for slope matching between the linear and saturation regions of the MOSFET output current-voltage curves. Four different sizes of transistors that cover a rectangular-shaped region of the channel length-width plane are analyzed.

Fast, simple and efficient supramolecular solvent-based microextraction of mecoprop and dichlorprop in soils prior to their enantioselective determination by liquid chromatography-tandem mass spectrometry.

PubMed

Caballo, C; Sicilia, M D; Rubio, S

2014-02-01

A simple, sensitive, rapid and economic method was developed for the quantification of enantiomers of chiral pesticides as mecoprop (MCPP) and dichlorprop (DCPP) in soil samples using supramolecular solvent-based microextraction (SUSME) combined with liquid chromatography coupled to mass spectrometry (LC-MS/MS). SUSME has been described for the extraction of chiral pesticides in water, but this is firstly applied to soil samples. MCPP and DCPP are herbicides widely used in agriculture that have two enantiomeric forms (R- and S-) differing in environmental fate and toxicity. Therefore, it is essential to have analytical methods for monitoring individual DCPP and MCPP enantiomers in environmental samples. MCPP and DCPP were extracted in a supramolecular solvent (SUPRAS) made up of dodecanoic acid aggregates, the extract was dried under a nitrogen stream, the two herbicides dissolved in acetate buffer and the aqueous extract directly injected in the LC-MS/MS system. The recoveries obtained were independent of soil composition and age of herbicide residues. The detection and quantitation limits of the developed method for the determination of R- and S-MCPP and R- and S-DCPP in soils were 0.03 and 0.1 ng g(-1), respectively, and the precision, expressed as relative standard deviation (n=6), for enantiomer concentrations of 5 and 100 ng g(-1) were in the ranges 4.1-6.1% and 2.9-4.1%. Recoveries for soil samples spiked with enantiomer concentrations within the interval 5-180 ng g(-1) and enantiomeric ratios (ERs) of 1, 3 and 9, ranged between 93 and 104% with standard deviations of the percent recovery varying between 0.3% and 6.0%. Because the SUPRAS can solubilize analytes through different type of interactions (dispersion, dipole-dipole and hydrogen bonds), it could be used to extract a great variety of pesticides (including both polar and non-polar) in soils. © 2013 Published by Elsevier B.V.

A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

PubMed

Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

2013-07-26

A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Biosynthesis of silver nanoparticles using fresh extracts of Tridax procumbens linn.

PubMed

Bhati-Kushwaha, Himakshi

2014-04-01

A simple and eco-friendly method for the synthesis of biogenic nanoparticles (NP's) using an aqueous solution of T. procumbens fresh plant extract (leaf and stem) as a bioreductant is reported. The prepared biogenic nanoparticles were well characterized using U.V. visible spectroscopy, scanning electron microscopy, X-ray diffraction and Fourier-transform infrared spectroscopy. The particles were confirmed to be elemental crystal by X-ray diffraction. The potential applications of biosynthesized nanoparticles as antimicrobial (antibacterial and antifungal) against pathogens Escherichia coli, Vibrio cholerae, Aspergillus niger and Aspergillusflavus were demonstrated.

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.

A simple method of DNA isolation from jute (Corchorus olitorius) seed suitable for PCR-based detection of the pathogen Macrophomina phaseolina (Tassi) Goid.

PubMed

Biswas, C; Dey, P; Satpathy, S; Sarkar, S K; Bera, A; Mahapatra, B S

2013-02-01

A simple method was developed for isolating DNA from jute seed, which contains high amounts of mucilage and secondary metabolites, and a PCR protocol was standardized for detecting the seedborne pathogen Macrophomina phaseolina. The cetyl trimethyl ammonium bromide method was modified with increased salt concentration and a simple sodium acetate treatment to extract genomic as well as fungal DNA directly from infected jute seed. The Miniprep was evaluated along with five other methods of DNA isolation in terms of yield and quality of DNA and number of PCR positive samples. The Miniprep consistently recovered high amounts of DNA with good spectral qualities at A260/A280. The DNA isolated from jute seed was found suitable for PCR amplification. Macrophomina phaseolina could be detected by PCR from artificially inoculated as well as naturally infected jute seeds. The limit of PCR-based detection of M. phaseolina in jute seed was determined to be 0·62 × 10(-7) CFU g(-1) seed. © 2012 The Society for Applied Microbiology.

Simple detection of residual enrofloxacin in meat products using microparticles and biochips.

PubMed

Ha, Mi-Sun; Chung, Myung-Sub; Bae, Dong-Ho

2016-05-01

A simple and sensitive method for detecting enrofloxacin, a major veterinary fluoroquinolone, was developed. Monoclonal antibody specific for enrofloxacin was immobilised on a chip and fluorescent dye-labelled microparticles were covalently bound to the enrofloxacin molecules. Enrofloxacin in solution competes with the microparticle-immobilised enrofloxacin (enroMPs) to bind to the antibody on the chip. The presence of enrofloxacin was verified by detecting the fluorescence of enrofloxacin-bound microparticles. Under optimum conditions, a high dynamic range was achieved at enrofloxacin concentrations ranging from 1 to 1000 μg kg(-1). The limits of detection and quantification for standard solutions were 5 and 20 μg kg(-1) respectively, which are markedly lower than the maximum residue limit. Using simple extraction methods, recoveries from fortified beef, pork and chicken samples were 43.4-62.3%. This novel method also enabled approximate quantification of enrofloxacin concentration: the enroMP signal intensity decreased with increasing enrofloxacin concentration. Because of its sensitivity, specificity, simplicity and rapidity, the method described herein will facilitate the detection and approximate quantification of enrofloxacin residues in foods in a high-throughput manner.

Facile Separation of 5-O-Galloylquinic Acid from Chinese Green Tea Extract using Mesoporous Zirconium Phosphate.

PubMed

Ma, Yilong; Shang, Yafang; Zhu, Danye; Wang, Caihong; Zhong, Zhifeng; Xu, Ziyang

2016-05-01

5-O-Galloylquinic acid from green tea and other plants is attracting increasing attention for its antioxidant and antileishmanial bioactivities. It is always isolated using a silica column, a Sephadex column and high-performance liquid chromatography (HPLC) methods, which are either laborious or instrument dependent. To develop a new method to easily separate 5-O-galloylquinic acid. Mesoporous zirconium phosphate (m-ZrP) was prepared to conveniently separate 5-O-galloylquinic acid from Chinese green tea extract, and the target compound was easily obtained by simple steps of adsorption, washing and desorption. The effects of the green tea extraction conditions, extract concentrations, and m-ZrP adsorption/desorption dynamics on the 5-O-galloylquinic acid separation were evaluated. 5-O-Galloylquinic acid that was separated from a 70% ethanol extract of green tea was of moderate HPLC purity (92%) and recovery (88%), and an increased non-specific binding of epigallocatechin gallate (EGCG) on m-ZrP was observed in the diluted tea extract. The times for maximal adsorption of 5-O-galloylquinic acid in 70% ethanol extract and maximal desorption of 5-O-galloylquinic acid in 0.4% phosphoric acid solution were confirmed as 7 h and 5 h, respectively. A facile method to separate 5-O-galloylquinic acid from Chinese green tea extract using m-ZrP was established. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Determination of perfluorinated compounds in fish fillet homogenates: method validation and application to fillet homogenates from the Mississippi River.

PubMed

Malinsky, Michelle Duval; Jacoby, Cliffton B; Reagen, William K

2011-01-10

We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100±13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented. Copyright © 2010 Elsevier B.V. All rights reserved.

Simultaneous determination of four trace level endocrine disrupting compounds in environmental samples by solid-phase microextraction coupled with HPLC.

PubMed

Wang, Lingling; Zhang, Zhenzhen; Xu, Xu; Zhang, Danfeng; Wang, Fang; Zhang, Lei

2015-09-01

A simple, rapid, sensitive and effective method for the simultaneous determination of four endocrine disrupting compounds (EDCs) (bisphenol A (BPA), bisphenol F (BPF), bisphenol AF (BPAF) and bisphenol AP (BPAP)) in environment water samples based on solid-phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) was developed. Multi-wall carbon nanotubes (MWCNTs) adsorbents showed a good affinity to the target analytes. These compounds were rapidly extracted within 10 min. Various experimental parameters that could affect the extraction efficiencies had been investigated in detail. Under the optimum conditions, the enrichment factors of the method for the target EDCs were found to be 500. Satisfactory precision and accuracy of the method were obtained in a low concentration range of 2.0-500.0 ng mL(-1). The method detection limits were in the range of 0.10-0.30 ng mL(-1). The high pre-concentration rate and efficiency of the method ensure its successful application in extraction of trace EDCs from large volumes of environmental water samples. The extraction recoveries in real samples ranged from 85.3% to 102.5% with the relative standard deviations (n=5) less than 3.74%. Copyright © 2015 Elsevier B.V. All rights reserved.

Current Nucleic Acid Extraction Methods and Their Implications to Point-of-Care Diagnostics.

PubMed

Ali, Nasir; Rampazzo, Rita de Cássia Pontello; Costa, Alexandre Dias Tavares; Krieger, Marco Aurelio

2017-01-01

Nucleic acid extraction (NAE) plays a vital role in molecular biology as the primary step for many downstream applications. Many modifications have been introduced to the original 1869 method. Modern processes are categorized into chemical or mechanical, each with peculiarities that influence their use, especially in point-of-care diagnostics (POC-Dx). POC-Dx is a new approach aiming to replace sophisticated analytical machinery with microanalytical systems, able to be used near the patient, at the point of care or point of need . Although notable efforts have been made, a simple and effective extraction method is still a major challenge for widespread use of POC-Dx. In this review, we dissected the working principle of each of the most common NAE methods, overviewing their advantages and disadvantages, as well their potential for integration in POC-Dx systems. At present, it seems difficult, if not impossible, to establish a procedure which can be universally applied to POC-Dx. We also discuss the effects of the NAE chemicals upon the main plastic polymers used to mass produce POC-Dx systems. We end our review discussing the limitations and challenges that should guide the quest for an efficient extraction method that can be integrated in a POC-Dx system.

Simultaneous Determination of Crypto-Chlorogenic Acid, Isoquercetin, and Astragalin Contents in Moringa oleifera Leaf Extracts by TLC-Densitometric Method.

PubMed

Vongsak, Boonyadist; Sithisarn, Pongtip; Gritsanapan, Wandee

2013-01-01

Moringa oleifera Lamarck (Moringaceae) is used as a multipurpose medicinal plant for the treatment of various diseases. Isoquercetin, astragalin, and crypto-chlorogenic acid have been previously found to be major active components in the leaves of this plant. In this study, a thin-layer-chromatography (TLC-)densitometric method was developed and validated for simultaneous quantification of these major components in the 70% ethanolic extracts of M. oleifera leaves collected from 12 locations. The average amounts of crypto-chlorogenic acid, isoquercetin, and astragalin were found to be 0.0473, 0.0427, and 0.0534% dry weight, respectively. The method was validated for linearity, precision, accuracy, limit of detection, limit of quantitation, and robustness. The linearity was obtained in the range of 100-500 ng/spot with a correlation coefficient (r) over 0.9961. Intraday and interday precisions demonstrated relative standard deviations of less than 5%. The accuracy of the method was confirmed by determining the recovery. The average recoveries of each component from the extracts were in the range of 98.28 to 99.65%. Additionally, the leaves from Chiang Mai province contained the highest amounts of all active components. The proposed TLC-densitometric method was simple, accurate, precise, and cost-effective for routine quality controlling of M. oleifera leaf extracts.

Trace quantification of selected sulfonamides in aqueous media by implementation of a new dispersive solid-phase extraction method using a nanomagnetic titanium dioxide graphene-based sorbent and HPLC-UV.

PubMed

Izanloo, Maryam; Esrafili, Ali; Behbahani, Mohammad; Ghambarian, Mahnaz; Reza Sobhi, Hamid

2018-02-01

Herein, a new dispersive solid-phase extraction method using a nano magnetic titanium dioxide graphene-based sorbent in conjunction with high-performance liquid chromatography and ultraviolet detection was successfully developed. The method was proved to be simple, sensitive, and highly efficient for the trace quantification of sulfacetamide, sulfathiazole, sulfamethoxazole, and sulfadiazine in relatively large volume of aqueous media. Initially, the nano magnetic titanium dioxide graphene-based sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy and X-ray diffraction. Then, the sorbent was used for the sorption and extraction of the selected sulfonamides mainly through π-π stacking hydrophobic interactions. Under the established conditions, the calibration curves were linear over the concentration range of 1-200 μg/L. The limit of quantification (precision of 20%, and accuracy of 80-120%) for the detection of each sulfonamide by the proposed method was 1.0 μg/L. To test the extraction efficiency, the method was applied to various fortified real water samples. The average relative recoveries obtained from the fortified samples varied between 90 and 108% with the relative standard deviations of 5.3-10.7%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Current Nucleic Acid Extraction Methods and Their Implications to Point-of-Care Diagnostics

PubMed Central

Ali, Nasir; Rampazzo, Rita de Cássia Pontello; Krieger, Marco Aurelio

2017-01-01

Nucleic acid extraction (NAE) plays a vital role in molecular biology as the primary step for many downstream applications. Many modifications have been introduced to the original 1869 method. Modern processes are categorized into chemical or mechanical, each with peculiarities that influence their use, especially in point-of-care diagnostics (POC-Dx). POC-Dx is a new approach aiming to replace sophisticated analytical machinery with microanalytical systems, able to be used near the patient, at the point of care or point of need. Although notable efforts have been made, a simple and effective extraction method is still a major challenge for widespread use of POC-Dx. In this review, we dissected the working principle of each of the most common NAE methods, overviewing their advantages and disadvantages, as well their potential for integration in POC-Dx systems. At present, it seems difficult, if not impossible, to establish a procedure which can be universally applied to POC-Dx. We also discuss the effects of the NAE chemicals upon the main plastic polymers used to mass produce POC-Dx systems. We end our review discussing the limitations and challenges that should guide the quest for an efficient extraction method that can be integrated in a POC-Dx system. PMID:28785592

Sensitive diagnosis of cutaneous leishmaniasis by lesion swab sampling coupled to qPCR

PubMed Central

ADAMS, EMILY R.; GOMEZ, MARIA ADELAIDA; SCHESKE, LAURA; RIOS, RUBY; MARQUEZ, RICARDO; COSSIO, ALEXANDRA; ALBERTINI, AUDREY; SCHALLIG, HENK; SARAVIA, NANCY GORE

2015-01-01

SUMMARY Variation in clinical accuracy of molecular diagnostic methods for cutaneous leishmaniasis (CL) is commonly observed depending on the sample source, the method of DNA recovery and the molecular test. Few attempts have been made to compare these variables. Two swab and aspirate samples from lesions of patients with suspected CL (n = 105) were evaluated alongside standard diagnosis by microscopic detection of amastigotes or culture of parasites from lesion material. Three DNA extraction methods were compared: Qiagen on swab and aspirate specimens, Isohelix on swabs and Boil/Spin of lesion aspirates. Recovery of Leishmania DNA was evaluated for each sample type by real-time polymerase chain reaction detection of parasitic 18S rDNA, and the diagnostic accuracy of the molecular method determined. Swab sampling combined with Qiagen DNA extraction was the most efficient recovery method for Leishmania DNA, and was the most sensitive (98%; 95% CI: 91–100%) and specific (84%; 95% CI: 64–95%) approach. Aspirated material was less sensitive at 80% (95% CI: 70–88%) and 61% (95% CI: 50–72%) when coupled to Qiagen or Boil-Spin DNA extraction, respectively. Swab sampling of lesions was painless, simple to perform and coupled with standardized DNA extraction enhances the feasibility of molecular diagnosis of CL. PMID:25111885

Novel methodology to isolate microplastics from vegetal-rich samples.

PubMed

Herrera, Alicia; Garrido-Amador, Paloma; Martínez, Ico; Samper, María Dolores; López-Martínez, Juan; Gómez, May; Packard, Theodore T

2018-04-01

Microplastics are small plastic particles, globally distributed throughout the oceans. To properly study them, all the methodologies for their sampling, extraction, and measurement should be standardized. For heterogeneous samples containing sediments, animal tissues and zooplankton, several procedures have been described. However, definitive methodologies for samples, rich in algae and plant material, have not yet been developed. The aim of this study was to find the best extraction protocol for vegetal-rich samples by comparing the efficacies of five previously described digestion methods, and a novel density separation method. A protocol using 96% ethanol for density separation was better than the five digestion methods tested, even better than using H 2 O 2 digestion. As it was the most efficient, simple, safe and inexpensive method for isolating microplastics from vegetal rich samples, we recommend it as a standard separation method. Copyright © 2018 Elsevier Ltd. All rights reserved.

Specific extraction of chromium as tetrabutylammonium-chromate and spectrophotometric determination by diphenylcarbazide: speciation of chromium in effluent streams.

PubMed

Noroozifar, M; Khorasani-Motlagh, M

2003-05-01

A very specific, selective, simple, and inexpensive procedure was developed for the speciation of CrVI and CrIII. This method is based on the quantitative extraction of chromate and CrIII (previously oxidized to CrVI) as a tetrabutylammonium-chromate ion-pair in methyl isobutyl ketone (MIBK), and then back extraction and preconcentration with an acidic diphenylcarbazide (DPC) solution. Back extraction was applied to achieve further preconcentration by a final factor of 20. The CrVI-DPC complex was determined in back-extract by a spectrophotometer at 548 nm. Under these extraction conditions, most of the probable concomitant cations and anions remained in the first inorganic phase. The calibration curve was linear up to 0.14 microg L(-1) of CrVI with a detection limit of 2.22 ng L(-1). The developed procedure was found to be suitable for the determination of the CrVI and CrIII species in various natural water samples with a relative standard deviation of better than 1.6%. The method was successfully applied to the speciation of chromium in spiked natural water samples, and also samples of effluent from a leather treatment plant.

A rapid and efficient assay for extracting DNA from fungi

USGS Publications Warehouse

Griffin, Dale W.; Kellogg, C.A.; Peak, K.K.; Shinn, E.A.

2002-01-01

Aims: A method for the rapid extraction of fungal DNA from small quantities of tissue in a batch-processing format was investigated. Methods and Results: Tissue (< 3.0 mg) was scraped from freshly-grown fungal isolates. The tissue was suspended in buffer AP1 and subjected to seven rounds of freeze/thaw using a crushed dry ice/ethanol bath and a boiling water bath. After a 30 min boiling step, the tissue was quickly ground against the wall of the microfuge tube using a sterile pipette tip. The Qiagen DNeasy Plant Tissue Kit protocol was then used to purify the DNA for PCR/ sequencing applications. Conclusions: The method allowed batch DNA extraction from multiple fungal isolates using a simple yet rapid and reliable assay. Significance and Impact of the Study: Use of this assay will allow researchers to obtain DNA from fungi quickly for use in molecular assays that previously required specialized instrumentation, was time-consuming or was not conducive to batch processing.

Rapid preconcentration method for the determination of azadirachtin-A and -B, nimbin and salannin in neem oil samples by using graphitised carbon solid phase extraction.

PubMed

Ramesh, A; Balasubramanian, M

1999-01-01

A simple and rapid method involving solid phase extraction and liquid chromatography for the determination of azadirachtin-A and -B, nimbin and salannin at nanogram levels in neem oil samples is presented. The neem oil samples are defatted and the compounds of interest extracted by mixing the sample with hexane and passing the hexane solution through a graphitised carbon black column. After washing the column with 2 ml of hexane, azadirachtin-A and -B, nimbin and salannin are eluted with 5 ml of acetonitrile and quantified using HPLC with UV detection. The recoveries of azadirachtin-A and -B, nimbin and salannin in fortified oil samples were 97.4-104.7%. The upper limit of quantification is up to 100 micrograms ml-1 without any additional clean-up and with little interference from lipids during the analysis by HPLC. The method was successfully applied to various neem oil samples collected from different locations in India.

Liquid chromatographic-diode-array detection multiresidue determination of rice herbicides in drinking and paddy-field water.

PubMed

Roehrs, Rafael; Zanella, Renato; Pizzuti, Ionara; Adaime, Martha B; Pareja, Lucía; Niell, Silvina; Cesio, María V; Heinzen, Horacio

2009-01-01

A sensitive, rapid, and simple multiresidue method for the simultaneous determination of six postemergence herbicides currently used in rice cultivation--metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium, and cyhalofop butyl--in drinking and paddy-field water is presented. Water samples were extracted with solid-phase extraction cartridges. Final determination was made by LC with diode-array detection. The extraction efficiencies of C18 and HLB cartridges were compared. The average recovery obtained for these compounds for the lowest spiked level (0.1 microg/L) varied from 70 to 122% for C18 and 75-119% for HLB, with RSDs of 11 and 8.3%, respectively. The method had good linearity, and the lower detection limit for the pesticides studied varied from 0.03 to 0.04 microg/L. The proposed method was also tested in paddy-field water, with recovery studies giving good results with low RSDs at 1.0 microg/L.

Steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry for fast determination of volatile components in jujube (Ziziphus jujuba Mill.) extract.

PubMed

Sun, Shi-Hao; Chai, Guo-Bi; Li, Peng; Xie, Jian-Ping; Su, Yue

2017-10-13

Jujube extract is commonly used as a food additive and flavoring. The unique jujube aroma and the mild sweet aroma of the extract are critical factors that determine product quality and affect consumer acceptability. The aroma changes with changes in the extraction condition, which is typically dependent on the characteristics of volatile oils in the extract. Despite their importance, the volatile oils of jujube extract have received less attention compared with the soluble components. So, an appropriate qualitative and quantitative method for determination of the volatile oils is vitally important for quality control of the product. A method coupling steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry (S3DE/GC-MS) was developed to determine the volatile components of jujube extract. Steam distillation was coupled with solvent extraction; the resulting condensate containing volatile components from jujube extract was drop-by-drop extracted using 2 mL of methyl tertiary butyl ether. The solvent served two purposes. First, the solvent extracted the volatile components from the condensate. Second, the volatile components were pre-concentrated by drop-by-drop accumulation in the solvent. As a result, the extraction, separation, and concentration of analytes in the sample were simultaneously completed in one step. The main parameters affecting the S3DE procedure, such as the water steam bubbling rate, extraction solvent volume, sample weight and S3DE time, were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R 2  ≥ 0.9887) and good repeatability (RSDs ≤ 10.35%, n = 5) for 16 analytes in spiked standard analyte samples were achieved. With the S3DE/GC-MS method, seventy-six volatile compounds from jujube extract were identified and the content of 16 compounds was measured. The results were similar to those from simultaneous distillation extraction. The developed method was simple, fast, effective, sensitive, and provided an overall profile of the volatile components in jujube extract. Thus, this method can be used to determine the volatile components of extracts. Graphical abstract The diagram of steam distillation/drop-by-drop extraction device.

Development of high-throughput multi-residue method for non-steroidal anti-inflammatory drugs monitoring in swine muscle by LC-MS/MS.

PubMed

Castilhos, Tamara S; Barreto, Fabiano; Meneghini, Leonardo; Bergold, Ana Maria

2016-07-01

A reliable and simple method for the detection and quantification of residues of 14 non-steroidal anti-inflammatory drugs and a metamizole metabolite in swine muscle was developed using liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The samples were extracted with acetonitrile (ACN) in solid-liquid extraction followed by a low-temperature partitioning (LLE-LTP) process at -20 ± 2°C. After evaporation to dryness, the residue was reconstituted with hexane and a mixture of water:acetonitrile (1:1). LC separation was achieved on a reversed-phase (RP18) column with gradient elution using water (phase A) and ACN (phase B) both containing 1 mmol l(-)(1) ammonium acetate (NH4COO) with 0.025% acetic acid. Analysis was carried out on a triple-quadrupole tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode using an electrospray interface in negative and positive mode in a single run. Method validation was performed according to the criteria of Commission Decision No. 2002/657/EC. The matrix effect and linearity were evaluated. Decision limit (CCα), detection capability (CCβ), accuracy and repeatability of the method are also reported. The proposed method proved to be simple, easy and adequate for high-throughput analysis and was applied to routine analysis by the Brazilian Ministry of Agriculture, Livestock and Food Supply.

Automatic QRS complex detection using two-level convolutional neural network.

PubMed

Xiang, Yande; Lin, Zhitao; Meng, Jianyi

2018-01-29

The QRS complex is the most noticeable feature in the electrocardiogram (ECG) signal, therefore, its detection is critical for ECG signal analysis. The existing detection methods largely depend on hand-crafted manual features and parameters, which may introduce significant computational complexity, especially in the transform domains. In addition, fixed features and parameters are not suitable for detecting various kinds of QRS complexes under different circumstances. In this study, based on 1-D convolutional neural network (CNN), an accurate method for QRS complex detection is proposed. The CNN consists of object-level and part-level CNNs for extracting different grained ECG morphological features automatically. All the extracted morphological features are used by multi-layer perceptron (MLP) for QRS complex detection. Additionally, a simple ECG signal preprocessing technique which only contains difference operation in temporal domain is adopted. Based on the MIT-BIH arrhythmia (MIT-BIH-AR) database, the proposed detection method achieves overall sensitivity Sen = 99.77%, positive predictivity rate PPR = 99.91%, and detection error rate DER = 0.32%. In addition, the performance variation is performed according to different signal-to-noise ratio (SNR) values. An automatic QRS detection method using two-level 1-D CNN and simple signal preprocessing technique is proposed for QRS complex detection. Compared with the state-of-the-art QRS complex detection approaches, experimental results show that the proposed method acquires comparable accuracy.

A fully validated method for the determination of lacosamide in human plasma using gas chromatography with mass spectrometry: application for therapeutic drug monitoring.

PubMed

Nikolaou, Panagiota; Papoutsis, Ioannis; Spiliopoulou, Chara; Voudris, Constantinos; Athanaselis, Sotiris

2015-01-01

A simple gas chromatographic method with mass spectrometry detection was developed and validated for the determination of lacosamide in human plasma. Lacosamide and the internal standard, levetiracetam-d6, were extracted from 200 μL plasma, by a solid-phase extraction through HF Bond Elut C18 columns, and derivatized using N-methyl-N-tert-butyldimethylsilyltrifluoroacetamide with 1% tert-butyldimethylsilylchloride in acetonitrile. The limit of quantification was found to be 0.20 μg/mL and the assay was linear up to 20.0 μg/mL with correlation coefficient ≥0.994. The intra- and interday precision values were <4.1% in terms of relative standard deviation (%) and the values of intra- and interday accuracy were found to be within -7.2 and 5.3% in terms of relative error (%). Absolute recovery of the method for lacosamide was determined at three concentration levels and ranged from 92.5 to 97.6%. The developed method uses small volumes of plasma and proved to be simple, rapid, and sensitive for the determination of lacosamide in plasma. This method can be used in routine every day analysis of plasma samples obtained from patients who follow respective antiepileptic treatment and for the investigation of clinical and forensic cases where lacosamide is involved. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Immunochromatographic assay of cadmium levels in oysters.

PubMed

Nishi, Kosuke; Kim, In-Hae; Itai, Takaaki; Sugahara, Takuya; Takeyama, Haruko; Ohkawa, Hideo

2012-08-15

Oysters are one of foodstuffs containing a relatively high amount of cadmium. Here we report on establishment of an immunochromatographic assay (ICA) method of cadmium levels in oysters. Cadmium was extracted with 0.l mol L(-1) HCl from oysters and cleaned up from other metals by the use of an anion-exchange column. The behavior of five metals Mn, Fe, Cu, Zn, and Cd was monitored at each step of extraction and clean-up procedure for the ICA method in an inductively coupled plasma-mass spectrometry (ICP-MS) analysis. The results revealed that a simple extraction method with the HCl solution was efficient enough to extract almost all of cadmium from oysters. Clean-up with an anion-exchange column presented almost no loss of cadmium adsorbed on the column and an efficient removal of metals other than cadmium. When a spiked recovery test was performed in the ICA method, the recovery ranged from 98% to 112% with relative standard deviations between 5.9% and 9.2%. The measured values of cadmium in various oyster samples in the ICA method were favorably correlated with those in ICP-MS analysis (r(2)=0.97). Overall results indicate that the ICA method established in the present study is an adequate and reliable detection method for cadmium levels in oysters. Copyright © 2012 Elsevier B.V. All rights reserved.

Simple method for self-referenced and lable-free biosensing by using a capillary sensing element.

PubMed

Liu, Yun; Chen, Shimeng; Liu, Qiang; Liu, Zigeng; Wei, Peng

2017-05-15

We demonstrated a simple method for self-reference and label free biosensing based on a capillary sensing element and common optoelectronic devices. The capillary sensing element is illuminated by a light-emitting diode (LED) light source and detected by a webcam. Part of gold film that deposited on the tubing wall is functionalized to carry on the biological information in the excited SPR modes. The end face of the capillary was monitored and separate regions of interest (ROIs) were selected as the measurement channel and the reference channel. In the ROIs, the biological information can be accurately extracted from the image by simple image processing. Moreover, temperature fluctuation, bulk RI fluctuation, light source fluctuation and other factors can be effectively compensated during detection. Our biosensing device has a sensitivity of 1145%/RIU and a resolution better than 5.287 × 10 -4 RIU, considering a 0.79% noise level. We apply it for concanavalin A (Con A) biological measurement, which has an approximately linear response to the specific analyte concentration. This simple method provides a new approach for multichannel SPR sensing and reference-compensated calibration of SPR signal for label-free detection.

Development of a simple one-pot extraction method for various drugs and metabolites of forensic interest in blood by modifying the QuEChERS method.

PubMed

Matsuta, Shuntaro; Nakanishi, Keiko; Miki, Akihiro; Zaitsu, Kei; Shima, Noriaki; Kamata, Tooru; Nishioka, Hiroshi; Katagi, Munehiro; Tatsuno, Michiaki; Tsuboi, Kento; Tsuchihashi, Hitoshi; Suzuki, Koichi

2013-10-10

A rapid and convenient extraction method has been developed for the determination of various drugs and metabolites of forensic interest in blood by modifying the dispersive solid-phase extraction method "QuEChERS". The following 13 analytes with various chemical properties were used for the method development and its validation: amphetamine, methamphetamine, zolpidem, the carboxylate-form major metabolite of zolpidem M-1, flunitrazepam, 7-aminoflunitrazepam, phenobarbital, triazolam, α-hydroxytriazolam, brotizolam, α-hydroxybrotizolam, chlorpromazine, and promethazine. The modification of the QuEChERS method includes the use of relatively large amounts of inorganic salts in order to coagulate blood, which allows easy isolation of the organic extract phase. A combination of 100 mg anhydrous magnesium sulfate as a dehydrating agent, 50mg sodium chloride as a salting-out agent, and 500 μL acetonitrile containing 0.2% acetic acid as the organic solvent provided the optimum conditions for processing a 100 μL whole blood sample. The recoveries of the analytes spiked into whole blood at 0.5 μg/mL ranged between 59% and 93%. Although the addition of the graphitized carbon Envi-carb for cleanup decreased the recoveries of zolpidem and its carboxylate-form metabolite M-1, it was very effective in avoiding interferences by cholesterol. The present method can provide a rapid, effective, user-friendly, and relatively hygienic method for the simultaneous extraction of a wide range of drugs and metabolites in whole blood specimens. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

A novel HPLC-MS/MS method for the simultaneous determination of astemizole and its major metabolite in dog or monkey plasma and application to pharmacokinetics.

PubMed

Back, Hyun-moon; Lee, Jong-Hwa; Chae, Jung-woo; Song, Byungjeong; Seo, Joung-Wook; Yun, Hwi-yeol; Kwon, Kwang-il

2015-10-10

Astemizole (AST), a second-generation antihistamine, is metabolized to desmethyl astemizole (DEA), and although it has been removed from the market for inducing QT interval prolongation, it has reemerged as a potential anticancer and antimalarial agent. This report describes a novel high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneously determining the concentrations of AST and DEA in beagle dog and cynomolgus monkey plasma with simple preparation method and short retention time. Prior to HPLC analyses, the plasma samples were extracted with simple liquid-liquid extraction method. The isocratic mobile phase was 0.025% trifluoroacetic acid (TFA dissolved in acetonitrile) and 20 mM ammonium acetate (94:6) at a flow rate of 0.25 mL/min and diphenhydramine used as internal standard. In MS/MS analyses, precursor ions of the analytes were optimized as protonated molecular ions: [M+H](+). The lower limit of quantification of astemizole was 2.5 ng/mL in both species and desmethyl astemizole were 7.5 ng/mL and 10 ng/mL in dog and monkey plasma, respectively. The accuracy, precision, and stability of the method were in accordance with FDA guidelines for the validation of bioanalytical methods. Finally this validated method was successfully applied to a pharmacokinetic study in dogs and monkeys after oral administration of 10 mg/kg AST. Copyright © 2015 Elsevier B.V. All rights reserved.

Recovery of primary sporocysts in vivo in the Schistosoma mansoni/Biomphalaria glabrata model using a simple fixation method suitable for extraction of genomic DNA and RNA.

PubMed

Allienne, Jean-François; Théron, André; Gourbal, Benjamin

2011-09-01

Detailed studies of host/parasite interactions are currently limited because in situ gene sequencing or monitoring of parasite gene expression is so far limited to genes presenting a high loci copy number in the Schistosome genome or a high level of expression. Indeed, how to investigate the host parasite molecular interplay when parasites are not directly accessible in vivo? Here we describe a method to circumvent this problem and to analyze DNA and RNA of Schistosoma mansoni during the interaction with its intermediate snail host Biomphalaria glabrata. We propose a technique for improved DNA and RNA extraction from the intra-molluscan stage of the parasite recovered after fixation of infected snails in Raillet-Henry solution. The extractions can be used for genetic analysis, transcription studies and microsatellite genotyping. Copyright © 2011 Elsevier Inc. All rights reserved.

Dispersive liquid-liquid microextraction of phenolic compounds from vegetable oils using a magnetic ionic liquid.

PubMed

Zhu, Shuqiang; Wang, Lijun; Su, Along; Zhang, Haixia

2017-08-01

A novel method was developed for the determination of two endocrine-disrupting chemicals, bisphenol A and 4-nonylphenol, in vegetable oil by dispersive liquid-liquid microextraction followed by ultra high performance liquid chromatography with tandem mass spectrometry. Using a magnetic liquid as the microextraction solvent, several key parameters were optimized, including the type and volume of the magnetic liquid, extraction time, amount of dispersant, and the type of reverse extractant. The detection limits for bisphenol A and 4-nonylphenol were 0.1 and 0.06 μg/kg, respectively. The recoveries were 70.4-112.3%, and the relative standard deviations were less than 4.2%. The method is simple for the extraction of bisphenol A and 4-nonylphenol from vegetable oil and suitable for routine analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

PubMed Central

Çabuk, Hasan; Köktürk, Mustafa

2013-01-01

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

Validation of a simple liquid chromatographic method for determination and quantitation of residual ivermectin and doramectin in pig liver.

PubMed

Knold, Lone; Reitov, Marianne; Mortensen, Anna Birthe; Hansen-Møller, Jens

2002-01-01

A rapid and quantitative method for the extraction, derivatization, and liquid chromatography with fluorescence detection of ivermectin (IVM) and doramectin (DOM) residues in porcine liver was developed and validated. IVM and DOM were extracted from the liver samples with acetonitrile, the supernatant was evaporated to dryness at 37 degrees C under nitrogen, and the residue was reconstituted in 1-methylimidazole solution. After 2 min at room temperature, IVM and DOM were converted to a fluorescent derivative and then separated on a Hypersil ODS column. The derivatives of IVM and DOM were detected and quantitated with high specificity by fluorescence (excitation: 365 nm, emission: 475 nm). Abamectin was used as an internal standard. The mean extraction efficiencies from fortified samples (15 ng/g) were 75% for IVM and 70% for DOM. The limit of detection was 0.8 ng/g for both IVM and DOM.

Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments.

PubMed

Norambuena, Luis; Gras, Nuri; Contreras, Sergio

2013-08-15

A simple and rapid method for the detection and extraction of oxolinic acid, flumequine, florfenicol and oxytetracycline from marine sediments was developed and validated. The analytes were extracted from the marine sediment using a solution of oxalic acid diluted in methanol with sonication before detection by HPLC using a diode-array detector (florfenicol and oxytetracycline) and fluorescence (oxolinic acid and flumequine). The quantification limits (QL) were 100 ng/g for oxytetracycline and florfenicol and 5 ng/g for oxolinic acid and flumequine. The coefficients of variation of the repeatability and intermediate precision were less than 10% in all of the analytes. The calibration curves were linear between 50 and 500 ng/ml for oxytetracycline and florfenicol and 1 and 20 ng/ml for oxolinic acid and flumequine. The recuperation rate for the analytes was above 86%. Copyright © 2013 Elsevier Ltd. All rights reserved.

Isolation and identification of arctiin and arctigenin in leaves of burdock (Arctium lappa L.) by polyamide column chromatography in combination with HPLC-ESI/MS.

PubMed

Liu, Shiming; Chen, Kaoshan; Schliemann, Willibald; Strack, Dieter

2005-01-01

A simple method involving polyamide column chromatography in combination with HPLC-PAD and HPLC-ESI/MS for isolating and identifying two kinds of lignans, arctiin and arctigenin, in the leaves of burdock (Arctium lappa L.) has been established. After extraction of burdock leaves with 80% methanol, the aqueous phase of crude extracts was partitioned between water and chloroform and the aqueous phase was fractionated on a polyamide glass column. The fraction, eluting with 100% methanol, was concentrated and gave a white precipitate at 4 degrees C from which two main compounds were purified by semi-preparative HPLC. In comparison with the UV and ESI-MS spectra and the HPLC retention time of authentic standards, the compounds were determined to be arctiin and arctigenin. The extraction/separation technique was validated using an internal standard method.

Design of experiments for amino acid extraction from tobacco leaves and their subsequent determination by capillary zone electrophoresis.

PubMed

Hodek, Ondřej; Křížek, Tomáš; Coufal, Pavel; Ryšlavá, Helena

2017-03-01

In this study, we optimized a method for the determination of free amino acids in Nicotiana tabacum leaves. Capillary electrophoresis with contactless conductivity detector was used for the separation of 20 proteinogenic amino acids in acidic background electrolyte. Subsequently, the conditions of extraction with HCl were optimized for the highest extraction yield of the amino acids because sample treatment of plant materials brings some specific challenges. Central composite face-centered design with fractional factorial design was used in order to evaluate the significance of selected factors (HCl volume, HCl concentration, sonication, shaking) on the extraction process. In addition, the composite design helped us to find the optimal values for each factor using the response surface method. The limits of detection and limits of quantification for the 20 proteinogenic amino acids were found to be in the order of 10 -5 and 10 -4  mol l -1 , respectively. Addition of acetonitrile to the sample was tested as a method commonly used to decrease limits of detection. Ambiguous results of this experiment pointed out some features of plant extract samples, which often required specific approaches. Suitability of the method for metabolomic studies was tested by analysis of a real sample, in which all amino acids, except for L-methionine and L-cysteine, were successfully detected. The optimized extraction process together with the capillary electrophoresis method can be used for the determination of proteinogenic amino acids in plant materials. The resulting inexpensive, simple, and robust method is well suited for various metabolomic studies in plants. As such, the method represents a valuable tool for research and practical application in the fields of biology, biochemistry, and agriculture.

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

PubMed

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

2012-06-01

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

In vitro and in vivo evaluation of the antioxidant and prooxidant activity of phenolic compounds obtained from grape (Vitis vinifera) pomace.

PubMed

Cotoras, Milena; Vivanco, Herman; Melo, Ricardo; Aguirre, María; Silva, Evelyn; Mendoza, Leonora

2014-12-16

The antioxidant and/or prooxidant ability of extracts obtained from wine waste were analyzed using in vitro and in vivo assays. Cyclic voltammetry was used as the in vitro assay to determine the antioxidant and/or prooxidant properties and, the in vivo effect on mycelial growth of the fungus Botrytis cinerea was evaluated. In addition, the prooxidant activity was evaluated by intracellular oxidation of compound 2,7-dichlorodihydrofluorescein diacetate (DCFH-DA) in B. cinerea. The extracts used in this study were obtained from grape pomace of Cabernet Sauvignon, Carménère and Syrah varieties from the Misiones de Rengo Vineyard by simple extraction, using methanol/HCl 1% (v/v), ethanol 70% (v/v), or Soxhlet extraction. According to the results obtained, gallic acid was the most represented phenolic compound independent of grape variety and extraction method. In addition, vanillic acid; protocatechuic acid, syringic acid, quercetin and kaempferol were found in the extracts. From this study it was possible concluded that, depending of the method of extraction of the grape residues and the grape variety (Cabernet Sauvignon, Carménère and Syrah), the extracts showed antioxidant and/or prooxidant activity. However, no correlation can be established between the anodic oxidation potentials of the extracts and their effect on the fungus B. cinerea.

A simple isocratic HPLC method for the simultaneous determination of sinensetin, eupatorin, and 3'-hydroxy-5,6,7,4'-tetramethoxyflavone in Orthosiphon stamineus extracts.

PubMed

Yam, Mun Fei; Mohamed, Elsnoussi Ali Hussin; Ang, Lee Fung; Pei, Li; Darwis, Yusrida; Mahmud, Roziahanim; Asmawi, Mohd Zaini; Basir, Rusliza; Ahmad, Mariam

2012-08-01

Orthosiphon stamineus extracts contain three flavonoids (3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin) as bioactive substances. Previous reported high performance liquid chromatography- ultraviolet (HPLC-UV) methods for the determination of these flavonoids have several disadvantages, including unsatisfactory separation times and not being well validated according to International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) standard guidelines. A rapid, specific reversed-phase HPLC method with isocratic elution of acetonitrile: isopropyl alcohol: 20mM phosphate buffer (NaH(2)PO(4)) (30:15:55, v/v) (pH 3.5) at a flow-rate of 1ml/minute, a column temperature of 25°C, and ultraviolet (UV) detection at 340 nm was developed. The method was validated and applied for quantification of different types of O stamineus extracts and fractions. The method allowed simultaneous determination of 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin in the concentration range of 0.03052-250 μg/ml. The limits of detection and quantification, respectively, were 0.0076 and 0.061 μg/ml for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, 0.0153 and 0.122 μg/ml for sinensetin and 0.0305 and 0.122 μg/ml for eupatorin. The percent relative standard deviation (% RSD) values for intraday were 0.048-0.368, 0.025-0.135, and 0.05-0.476 for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin, respectively, and those for intraday precision were 0.333-1.688, 0.722-1.055, and 0.548-1.819, respectively. The accuracy for intraday were 91.25%-103.38%, 94.32%-109.56%, and 92.85%-109.70% for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin, respectively, and those for interday accuracy were 97.49%-103.92%, 103.58%-104.57%, and 103.9%-105.33%, respectively. The method was found to be simple, accurate and precise and is recommended for routine quality control analysis of O stamineus extract containing the three flavonoids as the principle components in the extract. Copyright © 2012. Published by Elsevier B.V.

Rapid mixed mode solid phase extraction method for the determination of acrylamide in roasted coffee by HPLC-MS/MS.

PubMed

Bortolomeazzi, Renzo; Munari, Marina; Anese, Monica; Verardo, Giancarlo

2012-12-15

In this work, a rapid and reliable purification method based on a single mixed solid phase extraction (SPE) column, for the determination of acrylamide in roasted coffee by liquid chromatography-tandem mass spectrometry, was developed. Deuterium labelled d(3)-acrylamide was used as internal standard. Acrylamide was extracted by 10 mL of water and the extract purified by a single SPE column consisting of 0.5 g of an in-house prepared mixture of C18, strong cation (SCX) and anion exchange (SAX) sorbents in the ratio 2/1.5/1.5 (w/w/w). The amount of the three sorbents was optimised in order to eliminate the main interfering compounds present in coffee extracts, such as melanoidins, trigonelline, chlorogenic acids and caffeine. The SPE procedure was very simple and consisted of pushing 1 mL of an aqueous coffee extract through the SPE column followed by 1 mL of water which was collected for the analysis. The method was tested on six samples of roasted coffee of different composition and roasting level. The repeatability of the method, expressed as relative standard deviation (n=6), was lower than 5%. The recovery of acrylamide at three spiked levels ranged from 92% to 95%. The limits of detection (LOD) and quantitation (LOQ) were 5 and 16 μg kg(-1), respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Noninvasive extraction of fetal electrocardiogram based on Support Vector Machine

NASA Astrophysics Data System (ADS)

Fu, Yumei; Xiang, Shihan; Chen, Tianyi; Zhou, Ping; Huang, Weiyan

2015-10-01

The fetal electrocardiogram (FECG) signal has important clinical value for diagnosing the fetal heart diseases and choosing suitable therapeutics schemes to doctors. So, the noninvasive extraction of FECG from electrocardiogram (ECG) signals becomes a hot research point. A new method, the Support Vector Machine (SVM) is utilized for the extraction of FECG with limited size of data. Firstly, the theory of the SVM and the principle of the extraction based on the SVM are studied. Secondly, the transformation of maternal electrocardiogram (MECG) component in abdominal composite signal is verified to be nonlinear and fitted with the SVM. Then, the SVM is trained, and the training results are compared with the real data to ensure the effect of the training. Meanwhile, the parameters of the SVM are optimized to achieve the best performance so that the learning machine can be utilized to fit the unknown samples. Finally, the FECG is extracted by removing the optimal estimation of MECG component from the abdominal composite signal. In order to evaluate the performance of FECG extraction based on the SVM, the Signal-to-Noise Ratio (SNR) and the visual test are used. The experimental results show that the FECG with good quality can be extracted, its SNR ratio is significantly increased as high as 9.2349 dB and the time cost is significantly decreased as short as 0.802 seconds. Compared with the traditional method, the noninvasive extraction method based on the SVM has a simple realization, the shorter treatment time and the better extraction quality under the same conditions.

In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey.

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax

2015-07-01

A simple and fast method namely in-coupled syringe assisted octanol-water partition microextraction combined with high performance liquid chromatography (HPLC) has been developed for the extraction, preconcentration and determination of neonicotinoid insecticide residues (e.g. imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) in honey. The experimental parameters affected the extraction efficiency, including kind and concentration of salt, kind of disperser solvent and its volume, kind of extraction solvent and its volume, shooting times and extraction time were investigated. The extraction process was carried out by rapid shooting of two syringes. Therefore, rapid dispersion and mass transfer processes was created between phases, and thus affects the extraction efficiency of the proposed method. The optimum extraction conditions were 10.00 mL of aqueous sample, 10% (w/v) Na2SO4, 1-octanol (100µL) as an extraction solvent, shooting 4 times and extraction time 2min. No disperser solvent and centrifugation step was necessary. Linearity was obtained within the range of 0.1-3000 ngmL(-1), with the correlation coefficients greater than 0.99. The high enrichment factor of the target analytes was 100 fold and low limit of detection (0.25-0.50 ngmL(-1)) could be obtained. This proposed method has been successfully applied in the analysis of neonicotinoid residues in honey, and good recoveries in the range of 96.93-107.70% were obtained. Copyright © 2015 Elsevier B.V. All rights reserved.

Mapping axonal density and average diameter using non-monotonic time-dependent gradient-echo MRI

NASA Astrophysics Data System (ADS)

Nunes, Daniel; Cruz, Tomás L.; Jespersen, Sune N.; Shemesh, Noam

2017-04-01

White Matter (WM) microstructures, such as axonal density and average diameter, are crucial to the normal function of the Central Nervous System (CNS) as they are closely related with axonal conduction velocities. Conversely, disruptions of these microstructural features may result in severe neurological deficits, suggesting that their noninvasive mapping could be an important step towards diagnosing and following pathophysiology. Whereas diffusion based MRI methods have been proposed to map these features, they typically entail the application of powerful gradients, which are rarely available in the clinic, or extremely long acquisition schemes to extract information from parameter-intensive models. In this study, we suggest that simple and time-efficient multi-gradient-echo (MGE) MRI can be used to extract the axon density from susceptibility-driven non-monotonic decay in the time-dependent signal. We show, both theoretically and with simulations, that a non-monotonic signal decay will occur for multi-compartmental microstructures - such as axons and extra-axonal spaces, which were here used as a simple model for the microstructure - and that, for axons parallel to the main magnetic field, the axonal density can be extracted. We then experimentally demonstrate in ex-vivo rat spinal cords that its different tracts - characterized by different microstructures - can be clearly contrasted using the MGE-derived maps. When the quantitative results are compared against ground-truth histology, they reflect the axonal fraction (though with a bias, as evident from Bland-Altman analysis). As well, the extra-axonal fraction can be estimated. The results suggest that our model is oversimplified, yet at the same time evidencing a potential and usefulness of the approach to map underlying microstructures using a simple and time-efficient MRI sequence. We further show that a simple general-linear-model can predict the average axonal diameters from the four model parameters, and map these average axonal diameters in the spinal cords. While clearly further modelling and theoretical developments are necessary, we conclude that salient WM microstructural features can be extracted from simple, SNR-efficient multi-gradient echo MRI, and that this paves the way towards easier estimation of WM microstructure in vivo.

Mapping axonal density and average diameter using non-monotonic time-dependent gradient-echo MRI.

PubMed

Nunes, Daniel; Cruz, Tomás L; Jespersen, Sune N; Shemesh, Noam

2017-04-01

White Matter (WM) microstructures, such as axonal density and average diameter, are crucial to the normal function of the Central Nervous System (CNS) as they are closely related with axonal conduction velocities. Conversely, disruptions of these microstructural features may result in severe neurological deficits, suggesting that their noninvasive mapping could be an important step towards diagnosing and following pathophysiology. Whereas diffusion based MRI methods have been proposed to map these features, they typically entail the application of powerful gradients, which are rarely available in the clinic, or extremely long acquisition schemes to extract information from parameter-intensive models. In this study, we suggest that simple and time-efficient multi-gradient-echo (MGE) MRI can be used to extract the axon density from susceptibility-driven non-monotonic decay in the time-dependent signal. We show, both theoretically and with simulations, that a non-monotonic signal decay will occur for multi-compartmental microstructures - such as axons and extra-axonal spaces, which were here used as a simple model for the microstructure - and that, for axons parallel to the main magnetic field, the axonal density can be extracted. We then experimentally demonstrate in ex-vivo rat spinal cords that its different tracts - characterized by different microstructures - can be clearly contrasted using the MGE-derived maps. When the quantitative results are compared against ground-truth histology, they reflect the axonal fraction (though with a bias, as evident from Bland-Altman analysis). As well, the extra-axonal fraction can be estimated. The results suggest that our model is oversimplified, yet at the same time evidencing a potential and usefulness of the approach to map underlying microstructures using a simple and time-efficient MRI sequence. We further show that a simple general-linear-model can predict the average axonal diameters from the four model parameters, and map these average axonal diameters in the spinal cords. While clearly further modelling and theoretical developments are necessary, we conclude that salient WM microstructural features can be extracted from simple, SNR-efficient multi-gradient echo MRI, and that this paves the way towards easier estimation of WM microstructure in vivo. Copyright © 2017 Elsevier Inc. All rights reserved.

Use of extracts from oyster shell and soil for cultivation of Spirulina maxima.

PubMed

Jung, Joo-Young; Kim, Sunmin; Lee, Hansol; Kim, Kyochan; Kim, Woong; Park, Min S; Kwon, Jong-Hee; Yang, Ji-Won

2014-12-01

Calcium ion and trace metals play important roles in various metabolisms of photosynthetic organisms. In this study, simple methods were developed to extract calcium ion and micronutrients from oyster shell and common soil, and the prepared extracts were tested as a replacement of the corresponding chemicals that are essential for growth of microalgae. The oyster shell and soil were treated with 0.1 M sodium hydroxide or with 10 % hydrogen peroxide, respectively. The potential application of these natural sources to cultivation was investigated with Spirulina maxima. When compared to standard Zarrouk medium, the Spirulina maxima cultivated in a modified Zarrouk media with elements from oyster shell and soil extract exhibited increases in biomass, chlorophyll, and phycocyanin by 17, 16, and 64 %, respectively. These results indicate that the extracts of oyster shell and soil provide sufficient amounts of calcium and trace metals for successful cultivation of Spirulina maxima.

A surprising method for green extraction of essential oil from dry spices: Microwave dry-diffusion and gravity.

PubMed

Farhat, Asma; Fabiano-Tixier, Anne-Sylvie; Visinoni, Franco; Romdhane, Mehrez; Chemat, Farid

2010-11-19

Without adding any solvent or water, we proposed a novel and green approach for the extraction of secondary metabolites from dried plant materials. This "solvent, water and vapor free" approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. Microwave dry-diffusion and gravity (MDG) has been compared with a conventional technique, hydrodistillation (HD), for the extraction of essential oil from dried caraway seeds. Essential oils isolated by MDG were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by HD, but MDG was better than HD in terms of rapidity (45min versus 300min), energy saving, and cleanliness. The present apparatus permits fast and efficient extraction, reduces waste, avoids water and solvent consumption, and allows substantial energy savings. Copyright © 2010 Elsevier B.V. All rights reserved.

Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

PubMed

Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

2017-05-01

Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment. Copyright © 2017 Elsevier B.V. All rights reserved.

Feature extraction based on extended multi-attribute profiles and sparse autoencoder for remote sensing image classification

NASA Astrophysics Data System (ADS)

Teffahi, Hanane; Yao, Hongxun; Belabid, Nasreddine; Chaib, Souleyman

2018-02-01

The satellite images with very high spatial resolution have been recently widely used in image classification topic as it has become challenging task in remote sensing field. Due to a number of limitations such as the redundancy of features and the high dimensionality of the data, different classification methods have been proposed for remote sensing images classification particularly the methods using feature extraction techniques. This paper propose a simple efficient method exploiting the capability of extended multi-attribute profiles (EMAP) with sparse autoencoder (SAE) for remote sensing image classification. The proposed method is used to classify various remote sensing datasets including hyperspectral and multispectral images by extracting spatial and spectral features based on the combination of EMAP and SAE by linking them to kernel support vector machine (SVM) for classification. Experiments on new hyperspectral image "Huston data" and multispectral image "Washington DC data" shows that this new scheme can achieve better performance of feature learning than the primitive features, traditional classifiers and ordinary autoencoder and has huge potential to achieve higher accuracy for classification in short running time.

Validation of a quantitative NMR method for suspected counterfeit products exemplified on determination of benzethonium chloride in grapefruit seed extracts.

PubMed

Bekiroglu, Somer; Myrberg, Olle; Ostman, Kristina; Ek, Marianne; Arvidsson, Torbjörn; Rundlöf, Torgny; Hakkarainen, Birgit

2008-08-05

A 1H-nuclear magnetic resonance (NMR) spectroscopy method for quantitative determination of benzethonium chloride (BTC) as a constituent of grapefruit seed extract was developed. The method was validated, assessing its specificity, linearity, range, and precision, as well as accuracy, limit of quantification and robustness. The method includes quantification using an internal reference standard, 1,3,5-trimethoxybenzene, and regarded as simple, rapid, and easy to implement. A commercial grapefruit seed extract was studied and the experiments were performed on spectrometers operating at two different fields, 300 and 600 MHz for proton frequencies, the former with a broad band (BB) probe and the latter equipped with both a BB probe and a CryoProbe. The concentration average for the product sample was 78.0, 77.8 and 78.4 mg/ml using the 300 BB probe, the 600MHz BB probe and CryoProbe, respectively. The standard deviation and relative standard deviation (R.S.D., in parenthesis) for the average concentrations was 0.2 (0.3%), 0.3 (0.4%) and 0.3mg/ml (0.4%), respectively.

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.

Dispersive microextraction based on water-coated Fe₃O₄ followed by gas chromatography-mass spectrometry for determination of 3-monochloropropane-1,2-diol in edible oils.

PubMed

Zhao, Qin; Wei, Fang; Xiao, Neng; Yu, Qiong-Wei; Yuan, Bi-Feng; Feng, Yu-Qi

2012-06-01

In the present work, we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction (LPME) and magnetic solid-phase extraction (MSPE). In this method, trace amount of water directly absorbed on bare Fe₃O₄ to form water-coated Fe₃O₄ (W-Fe₃O₄) and rapid extraction can be achieved while W-Fe₃O₄ dispersed in the sample solution. The analyte adsorbed W-Fe₃O₄ can be easily collected and isolated from sample solution by application of a magnet. It was worth noting that in the proposed method water was used as extractant and Fe₃O₄ served as the supporter and retriever of water. The performance of the method was evaluated by extraction of 3-monochloropropane-1,2-diol (3-MCPD) from edible oils. The extracted 3-MCPD was then derived by a silylanization reagent (1-trimethylsilylimidazole) before gas chromatography-mass spectrometry (GC-MS) analysis. Several parameters that affected the extraction and derivatization efficiency were investigated. Our results showed that the limit of detection for 3-MCPD was 1.1 ng/g. The recoveries in spiked oil samples were in the range of 70.0-104.9% with the RSDs less than 5.6% (intra-day) and 6.4% (inter-day). Taken together, the simple, rapid and cost-effective method developed in current study, offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of traces of cobalt in soils: A field method

USGS Publications Warehouse

Almond, H.

1953-01-01

The growing use of geochemical prospecting methods in the search for ore deposits has led to the development of a field method for the determination of cobalt in soils. The determination is based on the fact that cobalt reacts with 2-nitroso-1-naphthol to yield a pink compound that is soluble in carbon tetrachloride. The carbon tetrachloride extract is shaken with dilute cyanide to complex interfering elements and to remove excess reagent. The cobalt content is estimated by comparing the pink color in the carbon tetrachloride with a standard series prepared from standard solutions. The cobalt 2-nitroso-1-naphtholate system in carbon tetrachloride follows Beer's law. As little as 1 p.p.m. can be determined in a 0.1-gram sample. The method is simple and fast and requires only simple equipment. More than 40 samples can be analyzed per man-day with an accuracy within 30% or better.

HPLC determination of strychnine and brucine in rat tissues and the distribution study of processed semen strychni.

PubMed

Chen, Jun; Hou, Ting; Fang, Yun; Chen, Zhi-peng; Liu, Xiao; Cai, Hao; Lu, Tu-lin; Yan, Guo-jun; Cai, Bao-chang

2011-01-01

A simple and low-cost HPLC method with UV absorbance detection was developed and validated to simultaneously determine strychnine and brucine, the most abundant alkaloids in the processed Semen Strychni, in rat tissues (kidney, liver, spleen, lung, heart, stomach, small intestine, brain and plasma). The tissue samples were treated with a simple liquid-liquid extraction prior to HPLC. The LOQs were in the range of 0.039-0.050 µg/ml for different tissue or plasma samples. The extraction recoveries varied from 71.63 to 98.79%. The linear range was 0.05-2 µg/ml with correlation coefficient of over 0.991. The intra- and inter-day precision was less than 15%. Then the method was used to measure the tissue distribution of strychnine and brucine after intravenous administration of 1 mg/kg crude alkaloids fraction (CAF) extracted from the processed Semen Strychni. The results revealed that strychnine and brucine possessed similar tissue distribution characterization. The highest level was observed in kidney, while the lowest level was found in brain. It was indicated that kidney might be the primary excretion organ of prototype strychnine and brucine. It was also deduced that strychnine and brucine had difficulty in crossing the blood-brain barrier. Furthermore, no long-term accumulation of strychnine and brucine was found in rat tissues.

Mixed hemimicelles solid-phase extraction based on sodium dodecyl sulfate (SDS)-coated nano-magnets for the spectrophotometric determination of Fingolomid in biological fluids

NASA Astrophysics Data System (ADS)

Azari, Zhila; Pourbasheer, Eslam; Beheshti, Abolghasem

2016-01-01

In this study, mixed hemimicelles solid-phase extraction (SPE) based on sodium dodecyl sulfate (SDS)-coated nano-magnets Fe3O4 was investigated as a novel method for the separation and determination of Fingolimod (FLM) in water, urine and plasma samples prior to spectrophotometeric determination. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory extraction recoveries can be produced. The main factors affecting the adsolubilization of analysts, such as pH, surfactant and adsorbent amounts, ionic strength, extraction time and desorption conditions were studied and optimized. Under the selected conditions, FLM has been quantitatively extracted. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries of 96%, 95% and 88% were observed for water, urine and plasma respectively. Proper linear behaviors over the investigated concentration ranges of 2-26, 2-17 and 2-13 mg/L with good coefficients of determination, 0.998, 0.997 and 0.995 were achieved for water, urine and plasma samples, respectively. To the best of our knowledge, this is the first time that a mixed hemimicelles SPE method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for monitoring of FLM in water and biological samples.

Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

2011-04-01

In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

PubMed

Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

2016-10-01

A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

Computer classification of remotely sensed multispectral image data by extraction and classification of homogeneous objects

NASA Technical Reports Server (NTRS)

Kettig, R. L.

1975-01-01

A method of classification of digitized multispectral images is developed and experimentally evaluated on actual earth resources data collected by aircraft and satellite. The method is designed to exploit the characteristic dependence between adjacent states of nature that is neglected by the more conventional simple-symmetric decision rule. Thus contextual information is incorporated into the classification scheme. The principle reason for doing this is to improve the accuracy of the classification. For general types of dependence this would generally require more computation per resolution element than the simple-symmetric classifier. But when the dependence occurs in the form of redundance, the elements can be classified collectively, in groups, therby reducing the number of classifications required.

Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent.

PubMed

Moyakao, Khwankaew; Santaladchaiyakit, Yanawath; Srijaranai, Supalax; Vichapong, Jitlada

2018-04-11

In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE). High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL -1 with a correlation of determination ( R² ) greater than 0.99. Limit of detection (LOD) ranged from 0.005 to 0.065 ng mL -1 , while limit of quantification (LOQ) ranged from 0.008 to 0.263 ng mL -1 . The enrichment factor (EF) ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

Hollow Fiber Supported Ionic Liquids Liquid-Phase Micro-extraction Followed by High-Performance Liquid Chromatography for the Determination of Polycyclic Aromatic Hydrocarbons in Milk Samples.

PubMed

Wang, Meng; Cheng, Chunsheng; Liu, Chunbo; Yang, Yaling

2018-01-01

A rapid, simple, reliable and efficient hollow fiber supported ionic liquids liquid-phase micro-extraction method (IL-HF-LPME) followed by high-performance liquid chromatography was successfully applied to the determination of four kinds of polycyclic aromatic hydrocarbons (PAHs) in milk samples. In the IL-HF-LPME method, a mixture of [OMIM]PF6 and lauric acid, in a ratio of 3:1, was immobilized in the pores of a polypropylene hollow fiber used as extraction solvent. A series of essential parameters influencing the extraction efficiency were investigated and optimized. Under the optimal conditions, the extraction equilibrium is achieved within 3 min, the good linearity was >0.9990, the limits of detection varied from 0.14 to 0.71 ng/mL, the limit of quantification values were between 0.4 and 1.8 ng/mL, and the relative standard deviations were in the range of 1.24-3.27% (n = 5). The proposed method was applied to analyze four PAHs in milk samples and recoveries were between 93.6 and 102.8%. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Gas-diffusion microextraction coupled with spectrophotometry for the determination of formaldehyde in cork agglomerates.

PubMed

Brandão, Pedro F; Ramos, Rui M; Valente, Inês M; Almeida, Paulo J; Carro, Antonia M; Lorenzo, Rosa A; Rodrigues, José A

2017-04-01

In this work, a simple methodology was developed for the extraction and determination of free formaldehyde content in cork agglomerate samples. For the first time, gas-diffusion microextraction was used for the extraction of volatile formaldehyde directly from samples, with simultaneous derivatization with acetylacetone (Hantzsch reaction). The absorbance of the coloured solution was read in a spectrophotometer at 412 nm. Different extraction parameters were studied and optimized (extraction temperature, sample mass, volume of acceptor solution, extraction time and concentration of derivatization reagent) by means of an asymmetric screening. The developed methodology proved to be a reliable tool for the determination of formaldehyde in cork agglomerates with the following suitable method features: low LOD (0.14 mg kg -1 ) and LOQ (0.47 mg kg -1 ), r 2  = 0.9994, and intraday and interday precision of 3.5 and 4.9%, respectively. The developed methodology was applied to the determination of formaldehyde in different cork agglomerate samples, and contents between 1.9 and 9.4 mg kg -1 were found. Furthermore, formaldehyde was also determined by the standard method EN 717-3 for comparison purposes; no significant differences between the results of both methods were observed. Graphical abstract Representation of the GDME system and its main components.

Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

PubMed

Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid-phase microextraction for rapid AP-MALDI and quantitation of nortriptyline in biological matrices.

PubMed

Wu, Hui-Fen; Ku, Hsin-Yi; Yen, Jyh-Hao

2008-07-01

A liquid-phase microextraction (LPME) method using a micropipette with disposable tips was demonstrated for coupling to atmospheric pressure MALDI-MS (AP-MALDI/MS) as a concentrating probe for rapid analysis and quantitative determination of nortriptyline drug from biological matrices including human urine and human plasma. This technique was named as micropipette extraction (MPE). The best optimized parameters of MPE coupled to AP-MALDI/MS experiments were extraction solvent, toluene; extraction time, 5 min; sample agitation rate, 480 rpm; sample pH, 7; salt concentration, 30%; hole size of micropipette tips, 0.61 mm (id); and matrix concentration, 1000 ppm using alpha-cyano-4-hydroxycinnamic acid (CHCA) as a matrix. Three detection modes of AP-MALDI/MS analysis including full scan, selective ion monitor (SIM), and selective reaction monitor (SRM) of MS/MS were also compared for the MPE performance. The results clearly demonstrated that the MS/MS method provides a wider linear range and lower LODs but poor RSDs than the full scan and SIM methods. The LOD values for the MPE under SIM and MS/MS modes in water, urine, and plasma were 6.26, 47.5, and 94.9 nM, respectively. The enrichment factors (EFs) of this current approach were 36.5-43.0 fold in water. In addition, compared to single drop microextraction (SDME) and LPME using a dual gauge microsyringe with a hollow fiber (LPME-HF) technique, the LODs acquired by the MPE method under MS/MS modes were comparable to those of LPME-HF and SDME but it is more convenient than both methods. The advantages of this novel method are simple, easy to use, low cost, and no contamination between experiments since disposable tips were used for the micropipettes. The MPE has the potential to be widely used in the future because it only requires a simple micropipette to perform all extraction processes. We believe that this technique can be a powerful tool for MALDI/MS analysis of biological samples and clinical applications.

Development, validation and application of an ultra high performance liquid chromatographic-tandem mass spectrometric method for the simultaneous detection and quantification of five different classes of veterinary antibiotics in swine manure.

PubMed

Van den Meersche, Tina; Van Pamel, Els; Van Poucke, Christof; Herman, Lieve; Heyndrickx, Marc; Rasschaert, Geertrui; Daeseleire, Els

2016-01-15

In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 μg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure. Copyright © 2015 Elsevier B.V. All rights reserved.

Deep eutectic solvent based gas-assisted dispersive liquid-phase microextraction combined with gas chromatography and flame ionization detection for the determination of some pesticide residues in fruit and vegetable samples.

PubMed

Farajzadeh, Mir Ali; Sattari Dabbagh, Masoumeh; Yadeghari, Adeleh

2017-05-01

In this study, a gas-assisted dispersive liquid-phase microextraction method using a deep eutectic solvent as the extraction solvent combined with gas chromatography and flame ionization detection was developed for the extraction and determination of some pesticide residues in vegetable and fruit juice samples. In this method, choline chloride and 4-chlorophenol at a molar ratio of 1:2 were mixed. By heating and vortexing, a clear, water-immiscible, and homogeneous liquid was formed. The obtained deep eutectic solvent was added to an aqueous solution of the analytes in a conical test tube. Air was bubbled into the aqueous solution and a cloudy solution was obtained. During this step, the analytes were extracted into the fine droplets of the extraction solvent. After centrifugation, an aliquot of the settled phase was injected into the separation system. Under the optimum extraction conditions, enrichment factors, and extraction recoveries were obtained in the ranges of 247-355 and 49-71%, respectively. The obtained values for the limits of detection and quantification were in the ranges of 0.24-1.4 and 0.71-4.2 μg/L, respectively. The proposed method is simple, fast, efficient, and inexpensive. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel reverse phase high-performance liquid chromatography method for standardization of Orthosiphon stamineus leaf extracts

PubMed Central

Saidan, Noor Hafizoh; Aisha, Abdalrahim F.A.; Hamil, Mohd Shahrul Ridzuan; Majid, Amin Malik Shah Abdul; Ismail, Zhari

2015-01-01

Background: Orthosiphon stamineus Benth. (Lamiaceae) is a traditional medicinal plant which has been used in treating various ailments such as kidney diseases, bladder inflammation, arthritis and diabetes. The leaves contain high concentration of phenolic compounds, thus, rosmarinic acid (RA), 3’-hydroxy-5, 6, 7, 4’-tetramethoxyflavone (TMF), sinensetin (SIN) and eupatorin (EUP) were chosen as a marker compounds for standardization of various O. stamineus leaf extracts. Objective: The aim was to develop and validate a new high-performance liquid chromatography (HPLC) method for quantification of 4 marker compounds (RA, TMF, SIN, EUP) in various O. stamineus leaf extracts. Materials and Methods: The method was developed and validated using RP-HPLC-diode-array detection at 320 nm for accuracy, precision and limits of detection and was applied for quantification of it markers in five different extracts prepared in solvents with increasing polarity, using a gradient mobile phase 0.1% formic acid: Acetonitrile at a flow rate of 1 ml/min on reverse phase acclaim polar advantage II C18 column (3 μm, 3 × 150 mm) with 18 min separation time. Results: The developed method provided satisfactory precision, and the accuracy of this method was in the range of 90.2% to 105.5%. All of 4 compounds showed good linearity at R2 > 0.999. Conclusion: The developed method is a simple, cost effective with shorter run time (18 min) in comparison to previous methods (30 min) and utilization of environmental-friendly solvents system. Therefore, this method has the potential to replace currently used methods in the routine standardization work of O. stamineus extracts, raw materials and its commercial products. PMID:25598631

A simple method to separate red wine nonpolymeric and polymeric phenols by solid-phase extraction.

PubMed

Pinelo, Manuel; Laurie, V Felipe; Waterhouse, Andrew L

2006-04-19

Simple polyphenols and tannins differ in the way that they contribute to the organoleptic profile of wine and their effects on human health. Very few straightforward techniques to separate red wine nonpolymeric phenols from the polymeric fraction are available in the literature. In general, they are complex, time-consuming, and generate large amounts of waste. In this procedure, the separation of these compounds was achieved using C18 cartridges, three solvents with different elution strengths, and pH adjustments of the experimental matrices. Two full factorial 2(3) experimental designs were performed to find the optimal critical variables and their values, allowing for the maximization of tannin recovery and separation efficiency (SE). Nonpolymeric phenols such as phenolic acids, monomers, and oligomers of flavonol and flavan-3-ols and anthocyanins were removed from the column by means of an aqueous solvent followed by ethyl acetate. The polymeric fraction was then eluted with a combination of methanol/acetone/water. The best results were attained with 1 mL of wine sample, a 10% methanol/water solution (first eluant), ethyl acetate (second eluant), and 66% acetone/water as the polymeric phenols-eluting solution (third eluant), obtaining a SE of ca. 90%. Trials with this method on fruit juices also showed high separation efficiency. Hence, this solid-phase extraction method has been shown to be a simple and efficient alternative for the separation of nonpolymeric phenolic fractions and the polymeric ones, and this method could have important applications to sample purification prior to biological testing due to the nonspecific binding of polymeric phenolics to nearly all enzymes and receptor sites.

Integrated spectral and image analysis of hyperspectral scattering data for prediction of apple fruit firmness and soluble solids content

USDA-ARS?s Scientific Manuscript database

Spectral scattering is useful for assessing the firmness and soluble solids content (SSC) of apples. In previous research, mean reflectance extracted from the hyperspectral scattering profiles was used for this purpose since the method is simple and fast and also gives relatively good predictions. T...

Efficacy of a Simple Formulation Composed of Nematode-Trapping Fungi and Bidens pilosa var. radiata Scherff Aqueous Extracts (BPE) for Controlling the Southern Root-Knot Nematode

PubMed Central

Ajitomi, Atsushi; Taba, Satoshi; Ajitomi, Yoshino; Kinjo, Misa; Sekine, Ken-taro

2018-01-01

We tested a formulation composed of a mixture of Bidens pilosa var. radiata extract (BPE) and nematode-trapping fungi for its effects on Meloidogyne incognita. In earlier evaluations of the effects of plant extracts on the hyphal growth of 5 species of nematode-trapping fungi with different capture organs (traps), the growth of all species was slightly inhibited. However, an investigation on the number of capture organs and nematode-trapping rates revealed that Arthrobotrys dactyloides formed significantly more rings and nematode traps than those of the control. An evaluation of simple mixed formulations prepared using sodium alginate showed that nematodes were captured with all formulations tested. The simple mixed formulation showed a particularly high capture rate. Furthermore, in a pot test, although the effects of a single formulation made from the fungus or plant extract were acceptable, the efficacy of the simple mixed formulation against M. incognita root-knot formation was particularly high. PMID:29311429

[Simultaneous determination of 33 primary aromatic amines in polystyrene and polyethylene masterbatches for foods by ultra-performance liquid chromatography-tandem mass spectrometry

PubMed

Man, Zhengyin; Wang, Quanlin; Li, Hesheng; Zhang, Aizhi; Shen, Jian

2015-03-01

A comprehensive analytical method based on ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) has been developed for the simultaneous determination of 33 primary aromatic amines (PAAs) in polystyrene (PS) and polyethylene (PE) masterbatches for foods. The PS masterbatches were dissolved with dichloromethane, and methanol was added to precipitate after extraction by ultrasound extraction. Then the extract was purified by passing through a carbon graphite solid phase extraction column. The PE masterbatches were swelled and extracted with dichloromethane by ultrasound. The purified PS solution and PE extract were concentrated, and diluted to 2 mL with methanol-water (1:9, v/v), and filtered through the membranes of 0.22 µm before UPLC-MS/MS analysis. The analytes were separated on a BEH Phenyl column (100 mm x 2.1 mm, 1.7 µm), eluted by gradient with 0.07% (v/v) formic acid in methanol-water (1:9, v/v). The PAAs were detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode and quantified by the internal standard method. The separation conditions, fragment voltages and collision energies were optimized. The impacts of extraction times, extraction solvents and concentration methods on recoveries were studied. The limits of detection for the 33 primary aromatic amines were 6-10 µg/kg, and the limits of quantitation were 20-30 µg/kg. The mean recoveries of the two different masterbatch products at three spiked levels of 20, 100, 200 µg/kg were 61.3%-119.8%, and the relative standard deviations were 1.4%-14.8%. The experimental results indicated that the method is simple, rapid, sensitive, accurate, and can meet the related requirements for determination.

A marker-based watershed method for X-ray image segmentation.

PubMed

Zhang, Xiaodong; Jia, Fucang; Luo, Suhuai; Liu, Guiying; Hu, Qingmao

2014-03-01

Digital X-ray images are the most frequent modality for both screening and diagnosis in hospitals. To facilitate subsequent analysis such as quantification and computer aided diagnosis (CAD), it is desirable to exclude image background. A marker-based watershed segmentation method was proposed to segment background of X-ray images. The method consisted of six modules: image preprocessing, gradient computation, marker extraction, watershed segmentation from markers, region merging and background extraction. One hundred clinical direct radiograph X-ray images were used to validate the method. Manual thresholding and multiscale gradient based watershed method were implemented for comparison. The proposed method yielded a dice coefficient of 0.964±0.069, which was better than that of the manual thresholding (0.937±0.119) and that of multiscale gradient based watershed method (0.942±0.098). Special means were adopted to decrease the computational cost, including getting rid of few pixels with highest grayscale via percentile, calculation of gradient magnitude through simple operations, decreasing the number of markers by appropriate thresholding, and merging regions based on simple grayscale statistics. As a result, the processing time was at most 6s even for a 3072×3072 image on a Pentium 4 PC with 2.4GHz CPU (4 cores) and 2G RAM, which was more than one time faster than that of the multiscale gradient based watershed method. The proposed method could be a potential tool for diagnosis and quantification of X-ray images. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

A magnetic-based dispersive micro-solid-phase extraction method using the metal-organic framework HKUST-1 and ultra-high-performance liquid chromatography with fluorescence detection for determining polycyclic aromatic hydrocarbons in waters and fruit tea infusions.

PubMed

Rocío-Bautista, Priscilla; Pino, Verónica; Ayala, Juan H; Pasán, Jorge; Ruiz-Pérez, Catalina; Afonso, Ana M

2016-03-04

A hybrid material composed by the metal-organic framework (MOF) HKUST-1 and Fe3O4 magnetic nanoparticles (MNPs) has been synthetized in a quite simple manner, characterized, and used in a magnetic-assisted dispersive micro-solid-phase extraction (M-d-μSPE) method in combination with ultra-high-performance liquid chromatography (UHPLC) and fluorescence detection (FD). The application was devoted to the determination of 8 heavy polycyclic aromatic hydrocarbons (PAHs) in different aqueous samples, specifically tap water, wastewaters, and fruit tea infusion samples. The overall M-d-μSPE-UHPLC-FD method was optimized and validated. The method is characterized by: its simplicity in both the preparation of the hybrid material (simple mixing) and the magnetic-assisted approach (∼10min extraction time), the use of low sorbent amounts (20mg of HKUST-1 and 5mg of Fe3O4 MNPs), and the low organic solvent consumption in the overall M-d-μSPE-UHPLC-FD method (1.5mL of acetonitrile in the M-d-μSPE method and 2.8mL of acetonitrile in the UHPLC-FD run). The resulting method has high sensitivity, with LODs down to 0.8ngL(-1); adequate intermediate precision, with relative standard deviation values (RSD) always lower than 6.3% (being the range 5.9-9.0% in tap water for a spiked level of 45ngL(-1), 6.1-14% in wastewaters for a spiked level of 45ngL(-1), and 7.2-17% in fruit tea infusion samples for a spiked level of 45ngL(-1)); and adequate relative recoveries, with average values of 82% in tap water, and 94% and 75% in wastewater and fruit tea infusion samples, respectively, if using the proper matrix-matched calibration. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of the effect of extraction solvent and organ selection on the chemical profile of Astragalus spinosus using HPTLC- multivariate image analysis.

PubMed

Shawky, Eman; Selim, Dina A

2017-09-01

The evaluation of extraction protocols for untargeted and targeted metabolomics was implemented for root and aerial organs of Astragalus spinosus in this work. The efficiency and complementarity of commonly used extraction solvents, namely petroleum ether, methylene chloride, ethyl acetate and n-butanol were considered for method evaluation using chemometric techniques in conjunction with new, simple, and fast high performance thin layer chromatography (HPTLC) method for fingerprint analysis by extracting information from a digitalized HPTLC plate using ImageJ software. A targeted approach was furtherly implemented by developing and validating an HPTLC method allowing the quantification of three saponin glycosides. The results of untargeted and targeted principle component analysis (PCA) and hierarchical cluster analysis (HCA) revealed that the apparent saponins profile seems to depend on a combined effect of matrix composition and the properties of the selected solvent for extraction, where both the biological matrix of the investigated plant organs, as well as the extraction solvent can influence the precision of metabolite abundances. Although, the aerial part is frequently discarded as waste, it is shown hereby that it has similar chemical profile compared to the medicinal part, roots, yet a different extraction solvents pattern is recognized between the two organs which can be attributed to the differences in the composition, permeability or accessibility of the sample matrix/organ tissues, rather than the chemical structures of the detected metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a simple and valid method for the trace determination of phthalate esters in human plasma using dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Ebrahim, Karim; Poursafa, Parinaz; Amin, Mohammad Mehdi

2017-11-01

A new method was developed for the trace determination of phthalic acid esters in plasma using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry analysis. Plasma proteins were efficiently precipitated by trichloroacetic acid and then a mixture of chlorobenzene (as extraction solvent) and acetonitrile (as dispersive solvent) rapidly injected to clear supernatant using a syringe. After centrifuging, chlorobenzene sedimented at the bottom of the test tube. 1 μL of this sedimented phase was injected into the gas chromatograph for phthalic acid esters analysis. Different factors affecting the extraction performance, such as the type of extraction and dispersive solvent, their volume, extraction time, and the effects of salt addition were investigated and optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were satisfactory and ranged between 820-1020 and 91-97%, respectively. The linear range was wide (50-1000 ng/mL) and limit of detection was very low (1.5-2.5 ng/mL for all analytes). The relative standard deviations for analysis of 1 μg/mL of the analytes were between 3.2-6.1%. Salt addition showed no significant effect on extraction recovery. Finally, the proposed method was successfully utilized for the extraction and determination of the phthalic acid esters in human plasma samples and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

A Rapid and Simple Real-Time PCR Assay for Detecting Foodborne Pathogenic Bacteria in Human Feces.

PubMed

Hanabara, Yutaro; Ueda, Yutaka

2016-11-22

A rapid, simple method for detecting foodborne pathogenic bacteria in human feces is greatly needed. Here, we examined the efficacy of a method that employs a combination of a commercial PCR master mix, which is insensitive to PCR inhibitors, and a DNA extraction method which used sodium dodecyl benzene sulfonate (SDBS), and Tween 20 to counteract the inhibitory effects of SDBS on the PCR assay. This method could detect the target genes (stx1 and stx2 of enterohemorrhagic Escherichia coli, invA of Salmonella Enteritidis, tdh of Vibrio parahaemolyticus, gyrA of Campylobacter jejuni, ceuE of Campylobacter coli, SEA of Staphylococcus aureus, ces of Bacillus cereus, and cpe of Clostridium perfringens) in a fecal suspension containing 1.0 × 10 1 to 1.0 × 10 3 CFU/ml. Furthermore, the assay was neither inhibited nor influenced by individual differences among the fecal samples of 10 subjects or fecal concentration (40-160 mg/ml in the fecal suspension). When we attempted to detect the genes of pathogenic bacteria in 4 actual clinical cases, we found that this method was more sensitive than standard culture method. These results showed that this assay is a rapid, simple detection method for foodborne pathogenic bacteria in human feces.

Determination of Diethyl Phthalate and Polyhexamethylene Guanidine in Surrogate Alcohol from Russia

PubMed Central

Monakhova, Yulia B.; Kuballa, Thomas; Leitz, Jenny; Lachenmeier, Dirk W.

2011-01-01

Analytical methods based on spectroscopic techniques were developed and validated for the determination of diethyl phthalate (DEP) and polyhexamethylene guanidine (PHMG), which may occur in unrecorded alcohol. Analysis for PHMG was based on UV-VIS spectrophotometry after derivatization with Eosin Y and 1H NMR spectroscopy of the DMSO extract. Analysis of DEP was performed with direct UV-VIS and 1H NMR methods. Multivariate curve resolution and spectra computation methods were used to confirm the presence of PHMG and DEP in the investigated beverages. Of 22 analysed alcohol samples, two contained DEP or PHMG. 1H NMR analysis also revealed the presence of signals of hawthorn extract in three medicinal alcohols used as surrogate alcohol. The simple and cheap UV-VIS methods can be used for rapid screening of surrogate alcohol samples for impurities, while 1H NMR is recommended for specific confirmatory analysis if required. PMID:21647285

Determination of diethyl phthalate and polyhexamethylene guanidine in surrogate alcohol from Russia.

PubMed

Monakhova, Yulia B; Kuballa, Thomas; Leitz, Jenny; Lachenmeier, Dirk W

2011-01-01

Analytical methods based on spectroscopic techniques were developed and validated for the determination of diethyl phthalate (DEP) and polyhexamethylene guanidine (PHMG), which may occur in unrecorded alcohol. Analysis for PHMG was based on UV-VIS spectrophotometry after derivatization with Eosin Y and (1)H NMR spectroscopy of the DMSO extract. Analysis of DEP was performed with direct UV-VIS and (1)H NMR methods. Multivariate curve resolution and spectra computation methods were used to confirm the presence of PHMG and DEP in the investigated beverages. Of 22 analysed alcohol samples, two contained DEP or PHMG. (1)H NMR analysis also revealed the presence of signals of hawthorn extract in three medicinal alcohols used as surrogate alcohol. The simple and cheap UV-VIS methods can be used for rapid screening of surrogate alcohol samples for impurities, while (1)H NMR is recommended for specific confirmatory analysis if required.

Application of Focused Ultrasound-Assisted Extraction for the Quantification of Persistent Organic Pollutions in Liver Tissue of Giant Toad (Rhinella marina).

PubMed

Flores-Ramírez, R; Espinosa-Reyes, G; Cilia-López, V G; González-Mille, D J; Rodríguez-Aguilar, M; Díaz de León-Martínez, L; Díaz-Barriga, F

2017-02-01

A simple and rapid focused ultrasound extraction method was developed for the determination of Persistent Organic Pollutants (POPs) in liver tissue obtained of giant toad (Rhinella marina) using a gas chromatography coupled to a mass detector with electron impact ionization. The performed method for POPs, was validated in fortified matrix, showing linearity from the LOQ up to 100 ng/mL; LODs and LOQs for each compound were between 1.7 and 4.8 and 3.5-7.5 ng/mL, respectively. Recovery rates were among 79%-116% for POPs determined. Finally, the method was applied in liver samples of giant toads found in a malarial area in Mexico. The sensitivity of the proposed method was good enough to ensure reliable determination of target analytes at concentration levels commonly found in this kind of samples.

[Methods of eliminating alkaloids from the seeds of Lupinus mutabilis Sweet].

PubMed

Torres Tello, F; Nagata, A; Dreifuss Spiegel, W

1980-06-01

The basic purpose of this work was to find a simple and economic method to control and eliminate the presence of alkaloids, as detected by organoleptic or toxicity tests, in Lupinus mutabilis, S. (tarhui) seeds. Taking advantage of the physical and chemical properties of the seeds, they were subjected to four methods of extraction; b) chemical treatment; c) extraction with two solvents, and d) treatment with a modified water-heat process. The results indicated that the most adequate method was the water-heat modified treatment, which showed a yield of 85% and a debittering efficiency of 98.6%, figures which were above those obtained with any of the other treatments studied. The final product had a bland taste without traces of bitterness and a 32% concentration of protein in the kayra line. Amino acid content showed this product to have an unusual high lysine content.

A sensitive and efficient method for trace analysis of some phenolic compounds using simultaneous derivatization and air-assisted liquid-liquid microextraction from human urine and plasma samples followed by gas chromatography-nitrogen phosphorous detection.

PubMed

Farajzadeh, Mir Ali; Afshar Mogaddam, Mohammad Reza; Alizadeh Nabil, Ali Akbar

2015-12-01

In present study, a simultaneous derivatization and air-assisted liquid-liquid microextraction method combined with gas chromatography-nitrogen phosphorous detection has been developed for the determination of some phenolic compounds in biological samples. The analytes are derivatized and extracted simultaneously by a fast reaction with 1-flouro-2,4-dinitrobenzene under mild conditions. Under optimal conditions low limits of detection in the range of 0.05-0.34 ng mL(-1) are achievable. The obtained extraction recoveries are between 84 and 97% and the relative standard deviations are less than 7.2% for intraday (n = 6) and interday (n = 4) precisions. The proposed method was demonstrated to be a simple and efficient method for the analysis of phenols in biological samples. Copyright © 2015 John Wiley & Sons, Ltd.

Determination of Ethyl Carbamate in Chinese Yellow Rice Wine by Diatomaceous Earth Extraction and GC/MS Method.

PubMed

Wu, Pinggu; Zhang, Liqun; Shen, Xianghong; Wang, Liyuan; Zou, Yan; Zhang, Jing; Tan, Ying; Tang, Jun; Ma, Bingjie; Pan, Xiaodong; Jiang, Wei

2015-01-01

A sensitive and rapid analytical method based on alkaline diatomaceous earth extraction followed by GC/MS was developed for the quantitative determination of the toxic contaminant ethyl carbamate (EC) in yellow rice wines. The optimal extraction conditions were investigated. With the application of diatomaceous earth extraction, the damage of organic acids to the capillary column was greatly reduced. By using d5-EC as an internal standard for quantitative analysis of EC, the linearity of the calibration curves was good between 10 and 1000 ng/mL. The LOD and LOQ were 1.7 and 5.0 μg/kg, respectively. The spiked level of EC was 5.0-300 μg/kg, and the average recovery of the spikes was between 78.4 and 98.2%, with an RSD between 4.3 and 8.3%. Upon validation by five laboratories when spiked with 50, 100, and 300 μg/kg, the average respective recoveries were 102.9, 102.2, and 98.7% with a RSD between 0.7 and 8.1%. The validation results demonstrated that the method is fast, simple, selective, and suitable for the determination of EC in yellow rice wines.

Preconcentration and determination of ceftazidime in real samples using dispersive liquid-liquid microextraction and high-performance liquid chromatography with the aid of experimental design.

PubMed

Razmi, Rasoul; Shahpari, Behrouz; Pourbasheer, Eslam; Boustanifar, Mohammad Hasan; Azari, Zhila; Ebadi, Amin

2016-11-01

A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid-liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001-10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish.

PubMed

Tsai, Dung-Ying; Chen, Chien-Liang; Ding, Wang-Hsien

2014-07-01

A simple and effective method for the rapid determination of five salicylate and benzophenone-type UV absorbing substances in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by on-line silylation gas chromatography tandem mass spectrometry (GC-MS/MS). The parameters that affect the extraction efficiency were optimized using a Box-Behnken design method. The optimal extraction conditions involved dispersing 0.5g of freeze-dried powdered fish with 1.0g of Florisil using a mortar and pestle. This blend was then transferred to a solid-phase extraction (SPE) cartridge containing 1.0g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7mL of acetonitrile. The extract was derivatized on-line in the GC injection-port by reaction with a trimethylsilylating (TMS) reagent. The TMS-derivatives were then identified and quantitated by GC-MS/MS. The limits of quantitation (LOQs) were less than 0.1ng/g. Copyright © 2014 Elsevier Ltd. All rights reserved.

Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

PubMed

Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

2014-06-01

A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

Detection of defects on apple using B-spline lighting correction method

NASA Astrophysics Data System (ADS)

Li, Jiangbo; Huang, Wenqian; Guo, Zhiming

To effectively extract defective areas in fruits, the uneven intensity distribution that was produced by the lighting system or by part of the vision system in the image must be corrected. A methodology was used to convert non-uniform intensity distribution on spherical objects into a uniform intensity distribution. A basically plane image with the defective area having a lower gray level than this plane was obtained by using proposed algorithms. Then, the defective areas can be easily extracted by a global threshold value. The experimental results with a 94.0% classification rate based on 100 apple images showed that the proposed algorithm was simple and effective. This proposed method can be applied to other spherical fruits.