[show abstract][hide abstract] ABSTRACT: A simple and reliable liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed for carbendazim (MBC), thiophanate (TE), thiophanate-methyl (TM) and benomyl (BM) in agricultural products. These compounds were extracted from agricultural products with methanol after addition of sodium L-ascorbate. BM was hydrolyzed to MBC during the extraction with methanol. TE and TM were cyclized to ethyl 2-benzimidazole carbamate (EBC) and MBC by refluxing at 120 °C for 30 min with copper acetate in 50% acetic acid. MBC and EBC were cleaned up by an n-hexane wash and extraction with ethyl acetate and determined by LC-MS/MS. The mean recoveries from 10 agricultural products were in the range of 75.8-100.0%, and the relative standard deviations of 5 experiments were in the range of 1.5-9.2% at concentrations equal to the maximum residue limits (MRLs). The calibration curves were made by using commercial MBC and EBC as reference analytical standards without refluxing. The quantification limits were 0.01 mg/kg (as MBC), which is the uniform limit in the positive list system for agricultural chemical residues in foods in Japan.
Journal of the Food Hygienic Society of Japan (Shokuhin Eiseigaku Zasshi) 01/2011; 52(3):148-55. · 0.33 Impact Factor
[show abstract][hide abstract] ABSTRACT: A highly sensitive gas chromatographic-mass spectrometric (GC-MS) method was developed for dithiocarbamates (DTCs) and milneb in foods. DTCs and milneb were extracted from foods with cysteine-EDTA solution as sodium salts, and methylated with methyl iodide. Methyl derivatives of DTCs and milneb were cleaned up on a neutral alumina mini column and determined by GC-MS. The mean recoveries of DTCs and milneb were in the range of 72-120%, except for methiram. The quantification limits were 0.01 mg/kg (as CS(2)) in foods except tea (0.1 mg/kg as CS(2)). The developed method was applied to 10 compounds (4 dimethyldithiocarbamates, 3 ethylenebisdithiocarbamates, polycarbamates, propineb and milneb).
Journal of the Food Hygienic Society of Japan (Shokuhin Eiseigaku Zasshi) 01/2010; 51(5):213-9. · 0.33 Impact Factor
[show abstract][hide abstract] ABSTRACT: A novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for trace residue determination of bicozamycin (BZM) in livestock products and seafoods. BZM was extracted from a sample with acetonitrile-water (4 : 1), followed by a two-stage SPE enrichment and cleanup. The first stage involved a styrene-divinylbenzene copolymer cartridge (GL-Pak PLS-2), and the second stage involved a divinylbenzene-N-vinylpyrrolidone copolymer cartridge (Oasis HLB). The LC separation was performed on a C18 column using 0.01% formic acid-methanol (8 : 2) as the mobile phase and MS detection with negative ion electrospray ionization. The mean recoveries from swine muscle, liver, yellowtail, and milk fortified at the minimum residue limit (MRL) levels and 0.01 microg/g were >70%, and the relative standard deviations (RSDs) were <20%. Limits of quantitation (LOQs) ranged from 0.002 to 0.005 microg/g.
Journal of the Food Hygienic Society of Japan (Shokuhin Eiseigaku Zasshi) 04/2009; 50(2):52-7. · 0.33 Impact Factor
[show abstract][hide abstract] ABSTRACT: An efficient clean-up procedure was developed for the trace residue determination of tetracyclines (TCs) in dark-colored honeys. TCs were extracted from samples with McIlvaine buffer (pH 4.0) containing 0.01 mol/L Na(2)EDTA. The extracts were treated with both a polymeric cartridge (GL-Pak PLS-2) and a metal chelate affinity column (MCAC) preloaded with copper(II). TCs were eluted and analyzed by high-performance liquid chromatography (HPLC) using fluorescence detection. The method was evaluated for the determination of oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) in buckwheat honey, because its color is the darkest. The mean recoveries of OTC, TC and CTC from spiked samples, at three fortification levels, were >70%, and the relative standard deviations (RSDs) were <10%. Limits of quantitation (LOQs) of OTC, TC, and CTC were estimated to be 0.015 mg/kg, 0.019 mg/kg, and 0.024 mg/kg, respectively.
Journal of the Food Hygienic Society of Japan (Shokuhin Eiseigaku Zasshi) 06/2008; 49(3):196-203. · 0.33 Impact Factor
[show abstract][hide abstract] ABSTRACT: A novel liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method was developed for the trace residue determination of chloramphenicol (CAP) in bee pollen. CAP was extracted from bee pollen with a mixture of methanol and 1% metaphosphoric acid solution, followed by a 2-stage solid-phase extraction enrichment and cleanup. The first stage involved a polymeric cartridge, and the second stage involved an alumina neutral cartridge. The LC separation was performed on a C18 column with 10 mM ammonium formate-acetonitrile (7 + 3) as the mobile phase and MS detection with negative-ion electrospray ionization. CAP-d5 was used as the internal standard. The method was validated according to Commission Decision 2002/657/EC. The calibration curves were linear between 0.1 and 5.0 ng/mL, and overall recoveries ranged from 98 to 113%. Decision limits (CCalpha) ranged from 0.05 to 0.07 microg/kg, and detection capabilities (CCbeta) ranged from 0.08 to 0.12 microg/kg. The developed method was applied to 11 samples.
Journal of AOAC International 91(5):1103-9. · 1.23 Impact Factor