Search results for "Extraction"
showing 10 items of 2072 documents
Optimization of clean-up procedure for patulin determination in apple juice and apple purees by liquid chromatography
2009
Patulin (PAT) is a mycotoxin produced in fruits, mainly in apples, by several fungal species that can be carried into industrial apple juice by-products during factory processing. An analytical method for determination of PAT in apple juice and another one for determination of this compound in apple purees and apple compotes by liquid chromatography are proposed in the present paper. These methods have better precision and sensitivity than previously reported methods and focus mainly on extraction and clean-up. To accomplish analytical methods with higher accuracy, lower limits of detection and simpler procedures for application in quality control of the goods, different extraction and clea…
Determination of N -nitrosamines in cosmetic products by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and liquid chromatog…
2018
A new analytical method for the simultaneous determination of trace levels of seven prohibited N-nitrosamines (N-nitrosodimethylamine, N-nitrosoethylmethylamine, N-nitrosopyrrolidine, N-nitrosodiethylamine, N-nitrosopiperidine, N-nitrosomorpholine, and N-nitrosodiethanolamine) in cosmetic products has been developed. The method is based on vortex-assisted reversed-phase dispersive liquid-liquid microextraction, which allows the extraction of highly polar compounds, followed by liquid chromatography with mass spectrometry. The variables involved in the extraction process were studied to obtain the highest enrichment factor. Under the selected conditions, 75 μL of water as extraction solvent …
Optimization of Matrix Solid-Phase Dispersion method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial s…
2010
Abstract A method based on Matrix Solid-Phase Dispersion (MSPD) has been developed for the determination of 5 mycotoxins (ochratoxin A and aflatoxins B and G) in different cereals. Several dispersants, eluents and ratios were tested during the optimization of the process in order to obtain the best results. Finally, samples were blended with C 18 and the mycotoxins were extracted with acetonitrile. Regarding to matrix effects, the results clearly demonstrated the necessity to use a matrix-matched calibration to validate the method. Analyses were performed by liquid chromatography–triple quadrupole-tandem mass spectrometry (LC–QqQ-MS/MS). The recoveries of the extraction process ranged from …
Simple liquid chromatography assay for analyzing ochratoxin A in bovine milk
2008
Abstract Ochratoxin A (OTA) is a mycotoxin with teratogenic and carcinogenic properties. Animal intake of feedstuffs contaminated with OTA may cause that some residues may be found in bovine milk, therefore, its analysis requires a highly sensitive, simple and precise technique. This method is based on a liquid–liquid extraction with methanol, followed by filtration and extract concentration. Liquid chromatography coupled to fluorescence detection was used for OTA analysis. In this way, several impurities are filtered off and OTA is quantified with a mean recovery of 93.0 ± 7.4% and a limit of detection of 0.01 ng mL −1 . Therefore, this methodology allows a simple quantitative extraction o…
Extraction and analysis of ochratoxin A in bread using pressurised liquid extraction and liquid chromatography.
2005
A pressurised liquid extraction (PLE) method for the analysis of ochratoxin A (OTA) in bread samples is given. Parameters such as solvent, temperature, pressure and time were investigated thoroughly. The optimized PLE conditions were: methanol as extraction solvent, 80 degrees C, 2000 psi and a 5-min cycle. OTA was determined by liquid chromatography coupled with fluorescence detection and confirmed by methyl ester derivatization. Under these conditions OTA recovery is 92.3% with a RSD of 5%. Limits of detection and quantification were 0.02 and 0.06 microg/kg, respectively. The proposed method was applied to 20 bread samples, finding two positive samples with OTA levels below the maximum pe…
Determination of ochratoxin A in maize bread samples by LC with fluorescence detection.
2007
Ochratoxin A (OTA) is a secondary fungal metabolite produced by several moulds, mainly by Aspergillus ochraceus, A. carbonarius, A. niger and by Penicillium verrucosum. The present work shows the results of comparative studies using different procedures for the analysis of OTA in maize bread samples. The studied analytical methods involved extraction with different volumes of PBS/methanol, different extraction apparatus, and clean-up through immunoaffinity columns. The separation and identification were carried out by high-performance liquid chromatography with fluorescence detection. The optimized method for analysis of OTA in maize bread involved extraction with PBS:methanol (50:50), and …
Validating quantitative PCR assays for cell-free DNA detection without DNA extraction: Exercise induced kinetics in systemic lupus erythematosus pati…
2021
ABSTRACTCirculating cell-free DNA (cfDNA) has been investigated as a screening tool for many diseases. To avoid expensive and time-consuming DNA isolation, direct quantification PCR assays can be established. However, rigorous validation is required to provide reliable data in the clinical and non-clinical context. Considering International Organization for Standardization, as well as bioanalytical method validation guidelines we provide a comprehensive procedure to validate assays for cfDNA quantification from unpurified blood plasma. A 90 and 222 bp assay was validated to study the kinetics of cfDNA after exercise in patients with systemic lupus erythematosus. The assays showed ultra-low …
DETERMINATION OF PENTOBARBITAL IN BIOLOGICAL SAMPLES BY MICELLAR LIQUID CHROMATOGRAPHY
1999
A liquid chromatographic procedure for the determination of pentobarbital in urine and plasma samples is described. The proposed system uses a Spherisorb octadecyl-silane ODS-2 C18 analytical column, a guard column of similar characteristics, and a 0.02 M CTAB-15% 1-propanol at pH 7.5 mobile phase. The UV detector was set at 250 nm. Pentobarbital was isolated from urine and plasma samples by using a single solid phase extraction procedure with LMS cartridges. Mephobarbital was used as internal standard. Limits of detection were 0.53 μg/mL and 0.60 μg/mL in urine and plasma samples respectively. In both cases the coefficients of variation were lower than 6.5%, and the recoveries ranged betwe…
Determination of ascorbic acid in asparagus by differential pulse polarography
1995
A useful method for the determination of ascorbic acid in a vegetable product (asparagus) by differential pulse polarography has been set up and evaluated. Extraction and instrumental conditions were optimized. The analytical parameters are: linearity (0–18.18 μg/ml); detection limit (0.182 μg/ml); instrumental and method precision (2.77% and 4%, respectively); accuracy (96.9–113.4%). These data show that the method is sufficiently sensitive, reliable and accurate. It was also compared with the official fluorometric AOAC method.
FTIR determination of Aspartame and Acesulfame-K in tabletop sweeteners.
2004
Two different strategies for sweeteners determination in tabletop samples by Fourier transform middle-infrared (FTIR) spectrometry, an off-line and a fully mechanized extraction of Aspartame and Acesulfame-K with different mixtures of chloroform and methanol, have been developed. The off-line method involves the extraction of both active principles by sonication of samples with 25:75 v/v CHCl3/CH3OH and direct measurement of the peak height values at 1751 cm(-1), corrected using a baseline defined at 1850 cm(-1) for Aspartame, and measurement of the peak height at 1170 cm(-1) in the first-order derivative spectra, corrected by using a horizontal baseline established at 1850 cm(-1), for Aces…