The applicability of a rapid and easy multiresidue method for determination of pesticide residues in agricultural products by using liquid chromatography/tandem mass spectrometry (LC/MS/MS) was examined. Pesticide residues were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride. The extract was purified with a double-layered cartridge column (graphite carbon black/primary-secondary amine silica gel). After removal of the solvent, the extract was resolved in methanol-water and analyzed with LC/MS/MS. Recovery tests of 99 pesticide residues from 7 agricultural products were performed at 20 and 100 ng/g. Throughout all of the agricultural products tested, 47 pesticides exhibited satisfactory recoveries (70-120%) and relative standard deviations (<20%) at both concentrations. The time for processing of 12 samples to test solutions was approximately 2-3 h. This method could be useful for determination of pesticide residues in agricultural products.
"Residues were separated by LC/MS/ MS and the RSD was <20%. Because of the good separation capacity, the method was proposed for the determination of pesticide residues in agricultural products (Takatori et al., 2008). "
[Show abstract][Hide abstract] ABSTRACT: The newest results in the employment of carbon-based composites in various chromatographic techniques such as gas-liquid chromatography, high-performance liquid chromatography and electrically driven separation techniques for the separation, quantitative determination and identification of a wide variety of compounds in complicated matrices are compiled. The results are concisely described and critically evaluated. The future trends in the application of carbon-based compounds in the chromatographic separation methods are briefly discussed.
[Show abstract][Hide abstract] ABSTRACT: In this study, a simple, effective, and sensitive method has been developed for the quantitative residue analysis of cyhalofop-butyl and its metabolite cyhalofop acid in water and soil when kept under laboratory conditions. The content of cyholofop-butyl and cyhalofop acid in water and soil was analyzed by first purifying the compounds through liquid-liquid extraction and partitioning followed by Silica gel (adsorption) chromatography. Upon the completion of the purification step the residual levels were monitored through high-performance liquid chromatography (HPLC) using a UV absorbance detector. The recoveries of cyhalofop-butyl from three replicates spiked at two different concentrations ranged from 82.5 to 100.0% and from 66.7 to 97.9% in water and soil, respectively. The limit of detection and minimum detection level of cyhalofop-butyl in water and soil was 0.02 ppm and 10 ng, respectively. The recoveries of cyhalofop acid ranged from 80.7 to 104.8% in water and from 76.9 to 98.1 % in soil. The limit of detection of cyhalofop acid was 0.005 ppm in water and 0.01 ppm in soil, while the minimum detection level was 2 ng both in water and soil. The half-live of cyhalofop-butyl was 4.14 and 6.6 days in water and soil, respectively. The method was successfully applied to evaluate cyhalofop-butyl residues in water and soil applied aj. 30% emulsion, oil in water (EW) product.
[Show abstract][Hide abstract] ABSTRACT: Pesticide testing in foodstuffs is a challenging application for mass spectrometry (MS), since it implies simultaneous trace analysis of hundreds of compounds belonging to a many classes, preferably undertaken in one fast run. The appearance and the use of new, more polar pesticides has prompted the use of liquid chromatography electrospray ionization MS (LC-ESI-MS) instead of gas chromatography. Currently, large-scale multi-residue methods (LSMRMs) (i.e. covering over 80 analytes) for pesticide analysis are developed using LC with tandem MS (LC-MS2) with triple quadrupole mass analyzers or LC with time-of-flight MS (LC-TOF-MS).The present article provides a review of the most significant MRMs for determining pesticide residues in foodstuffs. We discuss the main features of LC-MS2and LC-TOF-MS instruments, including recently introduced advances in instrumentation. In addition, we describe the advantages and the pitfalls of these methods, together with examples of the application of LC-TOF-MS and LC-MS2 to large-scale screening, identification and quantitation of pesticides in foodstuffs.
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