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Enantioseparation and dissipation of acephate and its highly toxic metabolite methamidophos in pakchoi by supercritical fluid chromatography tandem mass spectrometry
Authors:Linjie Jiang  Yue Geng  Lu Wang  Yi Peng  Wei Jing  Yaping Xu  Xiaowei Liu
Institution:1. Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin, P. R. China

Key Laboratory for Environmental Factors Control of Agro-product Quality Safety, Ministry of Agriculture and Rural Affairs, Tianjin, P. R. China

National Reference Laboratory for Agricultural Testing, Tianjin, P. R. China;2. Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin, P. R. China;3. Shimadzu (China) Co., LTD. Beijing Branch, Beijing, P. R. China

Abstract:Acephate is widely used in crops as racemate. However, the enantioselective dissipation of acephate enantiomers has not been investigated in pakchoi. A sensitive and effective approach was established for determining residues of acephate and its highly toxic metabolite methamidophos enantiomers by supercritical fluid chromatography tandem mass spectrometry. Baseline separations for their enantiomers were achieved by using a Chiralcel OD-H column. The optimal chromatographic conditions were obtained as follows: CO2/ethanol (95/5) as mobile phase; flow rate, 3.0 mL/min; column temperature, 40°C. The mean recoveries (RSDs) of analytes were in the range of 77–83.1% (6.1–9.9%), 75.4–87.5% (9.3–13.2%), and 81.5–84.2% (7.1–13.4%) at three fortification levels (0.005, 0.05, and 0.5 mg/kg for each enantiomer) for interday assay (n = 18). The method was used to evaluate the enantioselective dissipation of acephate and methamidophos in pakchoi. S-acephate dissipated faster than R-acephate, while the concentration of R-methamidophos was higher than that of S-methamidophos during the entire study period. The results indicated that the R-enantiomer of acephate and methamidophos was preferentially enriched in pakchoi. The established analysis approach and the study data provided useful information for the rational use of acephate in agriculture.
Keywords:acephate  dissipation  enantioselective separation  methamidophos  pakchoi
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