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Kaushik Banerjee - One of the best experts on this subject based on the ideXlab platform.
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A simultaneous screening and quantitative method for the Multiresidue Analysis of pesticides in spices using ultra-high performance liquid chromatography-high resolution (Orbitrap) mass spectrometry
Journal of chromatography. A, 2017Co-Authors: Arnab Goon, Zareen Khan, Dasharath P. Oulkar, Raviraj Shinde, Suresh Gaikwad, Kaushik BanerjeeAbstract:Abstract A novel screening and quantitation method is reported for non-target Multiresidue Analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70–120%, and precision-RSDs
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optimization of a sample preparation method for Multiresidue Analysis of pesticides in tobacco by single and multi dimensional gas chromatography mass spectrometry
Journal of Chromatography A, 2014Co-Authors: Zareen Khan, Kaushik Banerjee, Sagar C Utture, Rakesh Kumar Ghosh, Rushali Girame, Manasi Gadgil, Damodar D Reddy, Nalli JohnsonAbstract:Abstract A selective and sensitive Multiresidue Analysis method, comprising 4 7pesticides, was developed and validated in tobacco matrix. The optimized sample preparation procedure in combination with gas chromatography mass spectrometry in selected-ion-monitoring (GC-MS/SIM) mode offered limits of detection (LOD) and quantification (LOQ) in the range of 3–5 and 7.5–15 ng/g, respectively, with recoveries between 70 and 119% at 50–100 ng/g fortifications. In comparison to the modified QuEChERS (Quick-Easy-Cheap-Effective-Rugged-Safe method: 2 g tobacco + 10 ml water + 10 ml acetonitrile, 30 min vortexing, followed by dispersive solid phase extraction cleanup), the method performed better in minimizing matrix co-extractives e.g. nicotine and megastigmatrienone. Ambiguity in Analysis due to co-elution of target analytes (e.g. transfluthrin-heptachlor) and with matrix co-extractives (e.g. δ-HCH-neophytadiene, 2,4-DDE-linolenic acid) could be resolved by selective multi-dimensional (MD)GC heart-cuts. The method holds promise in routine Analysis owing to noticeable efficiency of 27 samples/person/day.
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optimization of gas chromatography single quadrupole mass spectrometry conditions for Multiresidue Analysis of pesticides in grapes in compliance to eu mrls
Food Chemistry, 2013Co-Authors: Kaushik Banerjee, Sagar C Utture, Soma Dasgupta, Sumaiyya Mujawar, Pandurang G AdsuleAbstract:Abstract A single quadrupole GC–MS method was optimized for Multiresidue determination of 47 pesticides in grapes with limit of quantifications of each compound in compliance with the EU-MRL requirements. Sample preparation involved extraction of 10 g sample with 10 ml ethyl acetate (+10 g sodium sulphate) by homogenization at 15,000 rpm followed by centrifugation at 3000 rpm. The supernatant was cleaned by dispersive solid phase extraction with primary secondary amine and acidified with 0.1% formic acid. Residues were estimated in selected ion monitoring mode with programmable temperature vaporizer-large volume injection (8 μl). All the GC and MS parameters were thoroughly optimized to achieve satisfactory linearity ( R 2 > 0.99) within 0.01–0.25 mg kg −1 with minimum matrix interferences. Recoveries at 0.01 and 0.02 mg kg −1 were within 67–120% with associated precision RSD below 19%. The method was successfully applied for Analysis of the real world samples for incurred residues.
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Multiresidue Analysis of multiclass plant growth regulators in grapes by liquid chromatography tandem mass spectrometry
Journal of AOAC International, 2011Co-Authors: Dasharath P. Oulkar, Kaushik Banerjee, Manoj Ghaste, S D Ramteke, Dattatraya G Naik, Shubhangi B Patil, Manjusha R Jadhav, Pandurang G AdsuleAbstract:A selective and rapid Multiresidue Analysis method is presented for simultaneous estimation of 12 plant growth regulators (PGRs), namely, auxins (indol-3-acetic acid, indol-3-butyric acid, and naphthyl acetic acid), cytokinins (kinetin, zeatin, and 6-benzyladenine), gibberellic acid (GA3), abscisic acid, and synthetic compounds, namely, forchlorfenuron, paclobutrazole, isoprothiolane, and 2,4-dichlorophenoxy acetic acid (2,4-D) in bud sprouts and grape berries at the development stages of 2-3 and 6-8 mm diameters, which are the critical phases when exogenous application of PGRs may be necessary to achieve desired grape quality and yield. The sample preparation method involved extraction of plant material with acidified methanol (50%) by homogenization for 2 min at 15000 rpm. The pH of the extract was enhanced up to 6 by adding ammonium acetate, followed by homogenization and centrifugation. The supernatant extract was cleaned by SPE on an Oasis HLB cartridge (200 mg, 6 cc). The final extract was measured directly by LC/MS/MS with electrospray ionization in positive mode, except for 2,4-D, GA3, and abscisic acid extracts, which required Analysis in negative mode. Quantification by multiple reaction monitoring (MRM) was supported with full-scan mass spectrometric confirmation using "information-dependent acquisition" triggered with MRM to "enhanced product ionization" mode of the hybrid quadrupole-ion trap mass analyzer. The LOQ of the test analytes varied between 1 and 10 ng/g with associated recoveries of 80-120% and precision RSD <25% (n = 8). Significant matrix-induced signal suppression was recorded when the responses for pre- and postextraction spikes of analytes were compared; this could be resolved by using matrix-matched calibration standards. The method could successfully be applied in analyzing incurred residue samples and would, therefore, be useful in precisely deciding the necessity and dose of exogenous applications of PGRs on the basis of measured endogenous levels.
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Multiresidue Analysis of 50 pesticides in grape pomegranate and mango by gas chromatography ion trap mass spectrometry
Journal of Agricultural and Food Chemistry, 2010Co-Authors: Rahul H Savant, Kaushik Banerjee, Sagar C Utture, Sangram H Patil, Soma Dasgupta, Manoj Ghaste, Pandurang G AdsuleAbstract:A selective and sensitive Multiresidue Analysis method is reported for simultaneous determination of 50 pesticides of different chemical classes in three commercially important fruits of different nature viz. grape, pomegranate, and mango. The sample preparation method involves extraction of a 10 g sample with 10 mL of ethyl acetate; cleanup by dispersive solid phase extraction with primary secondary amine (PSA, 25 mg) for grape and PSA + graphitized carbon black (25 + 5 mg) for pomegranate and mango; and determination by gas chromatography−ion trap mass spectrometry through multiple reaction monitoring (MRM). Sample preparation under acidified (pH 4) and cold (<4 °C) conditions, use of PTV-large volume injection (20 μL) through multibaffled liner and chromatographic separation on a short 10 m VF-5MS capillary column gave a satisfactory response for all of the analytes including relatively unstable compounds such as captan, captafol, folpet, endrine, and iprodione within 31.8 min. The limit of quantificat...
Pandurang G Adsule - One of the best experts on this subject based on the ideXlab platform.
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optimization of gas chromatography single quadrupole mass spectrometry conditions for Multiresidue Analysis of pesticides in grapes in compliance to eu mrls
Food Chemistry, 2013Co-Authors: Kaushik Banerjee, Sagar C Utture, Soma Dasgupta, Sumaiyya Mujawar, Pandurang G AdsuleAbstract:Abstract A single quadrupole GC–MS method was optimized for Multiresidue determination of 47 pesticides in grapes with limit of quantifications of each compound in compliance with the EU-MRL requirements. Sample preparation involved extraction of 10 g sample with 10 ml ethyl acetate (+10 g sodium sulphate) by homogenization at 15,000 rpm followed by centrifugation at 3000 rpm. The supernatant was cleaned by dispersive solid phase extraction with primary secondary amine and acidified with 0.1% formic acid. Residues were estimated in selected ion monitoring mode with programmable temperature vaporizer-large volume injection (8 μl). All the GC and MS parameters were thoroughly optimized to achieve satisfactory linearity ( R 2 > 0.99) within 0.01–0.25 mg kg −1 with minimum matrix interferences. Recoveries at 0.01 and 0.02 mg kg −1 were within 67–120% with associated precision RSD below 19%. The method was successfully applied for Analysis of the real world samples for incurred residues.
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Multiresidue Analysis of multiclass plant growth regulators in grapes by liquid chromatography tandem mass spectrometry
Journal of AOAC International, 2011Co-Authors: Dasharath P. Oulkar, Kaushik Banerjee, Manoj Ghaste, S D Ramteke, Dattatraya G Naik, Shubhangi B Patil, Manjusha R Jadhav, Pandurang G AdsuleAbstract:A selective and rapid Multiresidue Analysis method is presented for simultaneous estimation of 12 plant growth regulators (PGRs), namely, auxins (indol-3-acetic acid, indol-3-butyric acid, and naphthyl acetic acid), cytokinins (kinetin, zeatin, and 6-benzyladenine), gibberellic acid (GA3), abscisic acid, and synthetic compounds, namely, forchlorfenuron, paclobutrazole, isoprothiolane, and 2,4-dichlorophenoxy acetic acid (2,4-D) in bud sprouts and grape berries at the development stages of 2-3 and 6-8 mm diameters, which are the critical phases when exogenous application of PGRs may be necessary to achieve desired grape quality and yield. The sample preparation method involved extraction of plant material with acidified methanol (50%) by homogenization for 2 min at 15000 rpm. The pH of the extract was enhanced up to 6 by adding ammonium acetate, followed by homogenization and centrifugation. The supernatant extract was cleaned by SPE on an Oasis HLB cartridge (200 mg, 6 cc). The final extract was measured directly by LC/MS/MS with electrospray ionization in positive mode, except for 2,4-D, GA3, and abscisic acid extracts, which required Analysis in negative mode. Quantification by multiple reaction monitoring (MRM) was supported with full-scan mass spectrometric confirmation using "information-dependent acquisition" triggered with MRM to "enhanced product ionization" mode of the hybrid quadrupole-ion trap mass analyzer. The LOQ of the test analytes varied between 1 and 10 ng/g with associated recoveries of 80-120% and precision RSD <25% (n = 8). Significant matrix-induced signal suppression was recorded when the responses for pre- and postextraction spikes of analytes were compared; this could be resolved by using matrix-matched calibration standards. The method could successfully be applied in analyzing incurred residue samples and would, therefore, be useful in precisely deciding the necessity and dose of exogenous applications of PGRs on the basis of measured endogenous levels.
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Multiresidue Analysis of 50 pesticides in grape pomegranate and mango by gas chromatography ion trap mass spectrometry
Journal of Agricultural and Food Chemistry, 2010Co-Authors: Rahul H Savant, Kaushik Banerjee, Sagar C Utture, Sangram H Patil, Soma Dasgupta, Manoj Ghaste, Pandurang G AdsuleAbstract:A selective and sensitive Multiresidue Analysis method is reported for simultaneous determination of 50 pesticides of different chemical classes in three commercially important fruits of different nature viz. grape, pomegranate, and mango. The sample preparation method involves extraction of a 10 g sample with 10 mL of ethyl acetate; cleanup by dispersive solid phase extraction with primary secondary amine (PSA, 25 mg) for grape and PSA + graphitized carbon black (25 + 5 mg) for pomegranate and mango; and determination by gas chromatography−ion trap mass spectrometry through multiple reaction monitoring (MRM). Sample preparation under acidified (pH 4) and cold (<4 °C) conditions, use of PTV-large volume injection (20 μL) through multibaffled liner and chromatographic separation on a short 10 m VF-5MS capillary column gave a satisfactory response for all of the analytes including relatively unstable compounds such as captan, captafol, folpet, endrine, and iprodione within 31.8 min. The limit of quantificat...
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Multiresidue determination and uncertainty Analysis of 87 pesticides in mango by liquid chromatography tandem mass spectrometry
Journal of Agricultural and Food Chemistry, 2009Co-Authors: Kaushik Banerjee, Dasharath P. Oulkar, Sangram H Patil, Soma Dasgupta, Shubhangi B Patil, Manjusha R Jadhav, Sunita Bal, Pandurang G AdsuleAbstract:A liquid chromatography−tandem mass spectrometry (LC-MS/MS)-based method was optimized and validated for the Multiresidue Analysis of 87 pesticides in mango at the ≤10 ng g−1 level. The method invo...
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Multiresidue Analysis of 83 pesticides and 12 dioxin like polychlorinated biphenyls in wine by gas chromatography time of flight mass spectrometry
Journal of Chromatography A, 2009Co-Authors: Sangram H Patil, Dasharath P. Oulkar, Kaushik Banerjee, Rahul H Savant, Soma Dasgupta, Pandurang G Adsule, Shubhangi B Patil, Manjusha R Jadhav, M B DeshmukhAbstract:Abstract A Multiresidue method is described for simultaneous estimation of 83 pesticides and 12 dioxin-like polychlorinated biphenyls (PCBs) in red and white wines. The samples (20 mL wine, acidified with 20 mL 1% HCl) were extracted with 10 mL ethyl acetate (+20 g sodium sulphate) and cleaned by dispersive solid-phase extraction (DSPE) with anhydrous calcium chloride and Florisil successively. The final extract (5 mL) was solvent exchanged to 1 mL of cyclohexane:ethyl acetate (9:1), further cleaned by DSPE with 25 mg primary secondary amine sorbent and analyzed by gas chromatography–time-of-flight mass spectrometry (GC–TOF-MS) within 31 min run time. The limits of quantification of most analytes were ≤10–20 μg/L. Acidification of wine prior to extraction prevented hydrolysis of organophosphorous pesticides as well as dicofol, whereas treatment with CaCl2 minimized the fatty acid co-extractives significantly. Solvent exchange to cyclohexane:ethyl acetate (9:1) further minimized the co-extractives. Recoveries at 5, 10 and 20 ng/mL were >80% for most analytes except cyprodinil, buprofezin and iprodione. The expanded uncertainties at 10 ng/mL were
Xiaowei Liu - One of the best experts on this subject based on the ideXlab platform.
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Multiresidue Analysis of over 200 pesticides in cereals using a quechers and gas chromatography tandem mass spectrometry based method
Food Chemistry, 2015Co-Authors: Zeying He, Lu Wang, Yi Peng, Ming Luo, Wenwen Wang, Xiaowei LiuAbstract:A simple and high-throughput Multiresidue pesticide Analysis method was developed and validated for 219 pesticides in cereals (corn, wheat flour and rice) based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure combined with gas chromatography–triple quadrupole mass spectrometry (GC–MS/MS). Different buffer system (acetate- and citrate-buffered) and sample to solvent ratios (sample amount) were compared in the modified QuEChERS procedure to get better recovery and clean-up results. The limits of quantification (LOQ) ranged between 5 and 50 μg kg−1, and for the majority of the pesticides the LOQ were 5 μg kg−1, which were below the regulatory maximum residue limits. The coefficient of determination (r2) was >0.99 within the calibration linearity range of 2–200 μg kg−1 for the majority of the pesticides. Most recoveries at 5, 10, 20, 50, 100 and 200 μg kg−1 were in the range 70–120% (n = 6) with associated RSDs < 20% indicating satisfactory accuracy.
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Multiresidue Analysis of 213 pesticides in leek and garlic using quechers based method and gas chromatography triple quadrupole mass spectrometry
Analytical and Bioanalytical Chemistry, 2015Co-Authors: Shanshan Chen, Lu Wang, Yi Peng, Ming Luo, Wenwen Wang, Xiaowei LiuAbstract:A simple and sensitive Multiresidue pesticide Analysis method was developed and validated for 213 pesticides in leek and garlic based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure combined with gas chromatography-triple quadrupole mass spectrometry. In the QuEChERS method, commercial extraction salt packet, dispersive solid-phase extraction adsorbent packet, and ceramic homogenizer were used to simplify the extraction procedure. The gas chromatography-tandem mass spectrometry (GC-MS/MS) parameters were optimized for Analysis of 213 pesticides within a 38-min run time with a limit of quantification for most of the pesticides at 2 μg kg−1. The coefficient of determination (r2) was >0.99 within the calibration linearity range of 2–400 μg kg−1. Most recoveries at 2, 5, 10, 20, 50, 100, and 200 μg kg−1 were in the range of 70–120 % (n = 6) with associated relative standard deviations (RSDs) of <20 %, indicating satisfactory precision. Real leek and garlic samples were analyzed for method application.
Jon W Wong - One of the best experts on this subject based on the ideXlab platform.
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Perspectives on Liquid Chromatography–High-Resolution Mass Spectrometry for Pesticide Screening in Foods
2018Co-Authors: Jon W Wong, Kai Zhang, Douglas G Hayward, Jian Wang, Willis Chow, Roland Carlson, Zhengwei Jia, James S. ChangAbstract:This perspective discusses the use of liquid chromatography coupled with high-resolution mass spectrometry (LC–HRMS) for Multiresidue Analysis of pesticides in foods and agricultural commodities. HRMS has the important distinction and advantage of mass-resolving power and, therefore, requires different concepts, experiments, and guidance for screening, identification, and quantitation of pesticides in complex food matrices over triple quadrupole mass spectrometry. HRMS approaches for pesticide screening, including full-scan experiments in conjunction with tandem mass spectrometry (MS/MS) experiments, are described. This approach results in the generation of chromatographic retention times and high-resolution mass spectra with accurate mass measurements that can be used to create compound databases. New data processing tools can create an efficient and optimized screening approach that can speed the Analysis and identification of compounds, reduce the need for chemical standards, and harmonize pesticide analytical procedures
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targeted Multiresidue Analysis of veterinary drugs in milk based powders using liquid chromatography tandem mass spectrometry lc ms ms
Journal of Agricultural and Food Chemistry, 2017Co-Authors: James B Wittenberg, Kelli A Simon, Jon W WongAbstract:An analytical method was developed and validated for the determination of 40 veterinary drugs in various milk-based powders. The method involves acetonitrile/water extraction, solid-phase filtration for lipid removal in fat-containing matrices, and Analysis using liquid chromatography–tandem mass spectrometry (LC-MS/MS). The limits of quantitation (LOQ) ranged from 0.02 to 82 ng/g. Acceptable recoveries (70–120%, RSD < 20%) were reached for 40 of 52 target compounds at three fortification levels in nonfat milk powder. Similar results were obtained for whole milk powder, milk protein concentrate, whey protein concentrate, and whey protein isolate. This new method will allow for better monitoring of a wide range of veterinary drugs in milk-based powders.
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multi mycotoxin Analysis of finished grain and nut products using high performance liquid chromatography triple quadrupole mass spectrometry
Journal of Agricultural and Food Chemistry, 2013Co-Authors: Chiading Liao, Jon W Wong, Kai Zhang, Douglas G Hayward, Nathaniel S Lee, Mary W TrucksessAbstract:Mycotoxins in foods have long been recognized as potential health hazards due to their toxic and carcinogenic properties. A simple and rapid method was developed to detect 26 mycotoxins (aflatoxins, ochratoxins, fumonisins, trichothecenes, and ergot alkaloids) in corn, rice, wheat, almond, peanut, and pistachio products using high-performance liquid chromatography-triple-quadrupole mass spectrometry. Test portions of homogenized grain or nut products were extracted with acetonitrile/water (85:15, v/v), followed by high-speed centrifugation and dilution with water. Mean recoveries (± standard deviations) were 84 ± 6, 89 ± 6, 97 ± 9, 87 ± 12, 104 ± 16, and 92 ± 18% from corn, rice, wheat, almond, peanut, and pistachio products, respectively, and the matrix-dependent instrument quantitation limits ranged from 0.2 to 12.8 μg/kg, depending on the mycotoxin. Matrix effects, as measured by the slope ratios of matrix-matched and solvent-only calibration curves, revealed primarily suppression and were more pronounced in nuts than in grains. The measured mycotoxin concentrations in 11 corn and wheat reference materials were not different from the certified concentrations. Nineteen mycotoxins were identified and measured in 35 of 70 commercial grain and nut products, ranging from 0.3 ± 0.1 μg/kg (aflatoxin B1 in peanuts) to 1143 ± 87 μg/kg (fumonisin B1 in corn flour). This rapid and efficient method was shown to be rugged and effective for the Multiresidue Analysis of mycotoxins in finished grain and nut products.
Dasharath P. Oulkar - One of the best experts on this subject based on the ideXlab platform.
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A simultaneous screening and quantitative method for the Multiresidue Analysis of pesticides in spices using ultra-high performance liquid chromatography-high resolution (Orbitrap) mass spectrometry
Journal of chromatography. A, 2017Co-Authors: Arnab Goon, Zareen Khan, Dasharath P. Oulkar, Raviraj Shinde, Suresh Gaikwad, Kaushik BanerjeeAbstract:Abstract A novel screening and quantitation method is reported for non-target Multiresidue Analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70–120%, and precision-RSDs
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Multiresidue Analysis of multiclass plant growth regulators in grapes by liquid chromatography tandem mass spectrometry
Journal of AOAC International, 2011Co-Authors: Dasharath P. Oulkar, Kaushik Banerjee, Manoj Ghaste, S D Ramteke, Dattatraya G Naik, Shubhangi B Patil, Manjusha R Jadhav, Pandurang G AdsuleAbstract:A selective and rapid Multiresidue Analysis method is presented for simultaneous estimation of 12 plant growth regulators (PGRs), namely, auxins (indol-3-acetic acid, indol-3-butyric acid, and naphthyl acetic acid), cytokinins (kinetin, zeatin, and 6-benzyladenine), gibberellic acid (GA3), abscisic acid, and synthetic compounds, namely, forchlorfenuron, paclobutrazole, isoprothiolane, and 2,4-dichlorophenoxy acetic acid (2,4-D) in bud sprouts and grape berries at the development stages of 2-3 and 6-8 mm diameters, which are the critical phases when exogenous application of PGRs may be necessary to achieve desired grape quality and yield. The sample preparation method involved extraction of plant material with acidified methanol (50%) by homogenization for 2 min at 15000 rpm. The pH of the extract was enhanced up to 6 by adding ammonium acetate, followed by homogenization and centrifugation. The supernatant extract was cleaned by SPE on an Oasis HLB cartridge (200 mg, 6 cc). The final extract was measured directly by LC/MS/MS with electrospray ionization in positive mode, except for 2,4-D, GA3, and abscisic acid extracts, which required Analysis in negative mode. Quantification by multiple reaction monitoring (MRM) was supported with full-scan mass spectrometric confirmation using "information-dependent acquisition" triggered with MRM to "enhanced product ionization" mode of the hybrid quadrupole-ion trap mass analyzer. The LOQ of the test analytes varied between 1 and 10 ng/g with associated recoveries of 80-120% and precision RSD <25% (n = 8). Significant matrix-induced signal suppression was recorded when the responses for pre- and postextraction spikes of analytes were compared; this could be resolved by using matrix-matched calibration standards. The method could successfully be applied in analyzing incurred residue samples and would, therefore, be useful in precisely deciding the necessity and dose of exogenous applications of PGRs on the basis of measured endogenous levels.
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Multiresidue determination and uncertainty Analysis of 87 pesticides in mango by liquid chromatography tandem mass spectrometry
Journal of Agricultural and Food Chemistry, 2009Co-Authors: Kaushik Banerjee, Dasharath P. Oulkar, Sangram H Patil, Soma Dasgupta, Shubhangi B Patil, Manjusha R Jadhav, Sunita Bal, Pandurang G AdsuleAbstract:A liquid chromatography−tandem mass spectrometry (LC-MS/MS)-based method was optimized and validated for the Multiresidue Analysis of 87 pesticides in mango at the ≤10 ng g−1 level. The method invo...
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Multiresidue Analysis of 83 pesticides and 12 dioxin like polychlorinated biphenyls in wine by gas chromatography time of flight mass spectrometry
Journal of Chromatography A, 2009Co-Authors: Sangram H Patil, Dasharath P. Oulkar, Kaushik Banerjee, Rahul H Savant, Soma Dasgupta, Pandurang G Adsule, Shubhangi B Patil, Manjusha R Jadhav, M B DeshmukhAbstract:Abstract A Multiresidue method is described for simultaneous estimation of 83 pesticides and 12 dioxin-like polychlorinated biphenyls (PCBs) in red and white wines. The samples (20 mL wine, acidified with 20 mL 1% HCl) were extracted with 10 mL ethyl acetate (+20 g sodium sulphate) and cleaned by dispersive solid-phase extraction (DSPE) with anhydrous calcium chloride and Florisil successively. The final extract (5 mL) was solvent exchanged to 1 mL of cyclohexane:ethyl acetate (9:1), further cleaned by DSPE with 25 mg primary secondary amine sorbent and analyzed by gas chromatography–time-of-flight mass spectrometry (GC–TOF-MS) within 31 min run time. The limits of quantification of most analytes were ≤10–20 μg/L. Acidification of wine prior to extraction prevented hydrolysis of organophosphorous pesticides as well as dicofol, whereas treatment with CaCl2 minimized the fatty acid co-extractives significantly. Solvent exchange to cyclohexane:ethyl acetate (9:1) further minimized the co-extractives. Recoveries at 5, 10 and 20 ng/mL were >80% for most analytes except cyprodinil, buprofezin and iprodione. The expanded uncertainties at 10 ng/mL were
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optimization of separation and detection conditions for the Multiresidue Analysis of pesticides in grapes by comprehensive two dimensional gas chromatography time of flight mass spectrometry
Journal of Chromatography A, 2008Co-Authors: Kaushik Banerjee, Dasharath P. Oulkar, Rahul H Savant, Sangram H Patil, Soma Dasgupta, Shubhangi B Patil, Pandurang G AdsuleAbstract:Abstract A comprehensive GC×GC–TOFMS method was optimized for Multiresidue Analysis of pesticides using a combination of a non-polar (RTX-5MS, 10 m × 0.18 mm × 0.2 μm) and a polar capillary column (TR-50MS, 1 m × 0.1 mm × 0.1 μm), connected in series through a dual stage thermal modulator. The method resolved the co-elution problems as observed in full scan one-dimensional GC–MS Analysis and allowed chromatographic separation of 51 pesticides within 24 min run time with library-searchable mass spectrometric confirmation. Four pesticides, viz. chlorpyrifos-methyl, vinclozoline, parathion-methyl and heptachlor could be baseline separated on GC×GC, which were otherwise closely eluting and interfering each other's detection in 1 D GC–MS run. Similarly, it could be possible to separate myclobutanil, buprofezin, flusilazole and oxyfluorfen on GC×GC. Although in 1 D GC–MS, these closely eluting compounds could be identified through deconvolution algorithm and ‘peak-find’ option of the Chromatof ® software but the spectral purity significantly improved on GC×GC Analysis. Thorough optimization was accomplished for the oven temperature programming, ion source temperature and GC×GC parameters like modulation period, duration of hot pulses, modulation-offset temperature, acquisition rate, etc. to achieve best possible separation of the test compounds. The limit of detection significantly improved by 2–12 times on GC×GC–TOFMS against GC–TOFMS because of sharper and narrower peak shapes. The method was tested for grape matrix after preparing the samples using previously described method and recoveries of the entire test pesticides were within 70–110% at 10 ng/g level of fortification. GC×GC–TOFMS was found to be an excellent technique for library-based screening of pesticides with high accuracy and sensitivity.
