Search results for "Detection limit"
showing 10 items of 810 documents
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 …
Determination of total mercury in nuts at ultratrace level
2014
Abstract Total mercury, at μg kg−1 level, was determined in different types of nuts (cashew nut, Brazil nuts, almond, pistachio, peanut, walnut) using a direct mercury analyser after previous sample defatting and by cold vapour atomic fluorescence spectrometry. There is not enough sensitivity in the second approach to determine Hg in previously digested samples due to the strong matrix effect. Mercury levels in 25 edible nut samples from Brazil and Spain were found in the range from 0.6 to 2.7 μg kg−1 by using the pyrolysis of sample after the extraction of the nut fat. The accuracy of the proposed method was confirmed by analysing certified reference materials of Coal Fly Ash-NIST SRM 1633…
Simultaneous quantification of the main organic acids and carbohydrates involved in tomato flavour using capillary zone electrophoresis
2002
A capillary zone electrophoresis (CZE) procedure for the simultaneous determination of the major organic acids (oxalate, malate and citrate) and carbohydrates (fructose, glucose and sucrose) in Lycopersicon fruits is reported. Comparison of this method with routine HPLC methods indicates that the CZE method offers several attractive features (speed, resolution, sensitivity and cost) which significantly improve the determination of these compounds. Detection limits were better than 1.6 µg ml−1 for organic acids and from 13 to 24 µg ml−1 for carbohydrates; repeatabilities were better than 2.1% for migration times and between 1.4 and 7.3% for peak areas. The proposed protocol is very useful to…
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 …
Validated, non-destructive and environmentally friendly determination of cocaine in euro bank notes.
2005
A non-destructive, fast and environmentally friendly procedure has been developed for cocaine determination in euro bank notes. Cocaine was extracted with 15 ml methanol by vortex agitation during 5 min. The extract was evaporated and reconstituted in 0.5 ml methanol. GC-MS-MS analysis was performed using as precursor ion m/z 182.2, with an excitation energy voltage of 1.60 eV, being the product ions measured m/z 150.2 and 82.0. A limit of detection of 0.15 ng per note and a repeatability of 6%, established from the relative standard deviation, of a 1 ng ml(-1) level, were achieved. Recoveries of 101+/-2 and 98+/-3% were obtained for samples spiked with 100 and 10 microg respectively. Resul…
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…