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Enantioselective determination of acylamino acid fungicides in vegetables and fruits by chiral liquid chromatography coupled with tandem mass spectrometry
Authors:Zhang Hu  Wang Xinquan  Jin Lixia  Qian Mingrong  Wang Xiangyun  Xu Hao  Qi Peipei  Wang Qiang  Wang Minghua
Institution:Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences;, State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control; MOA Key Laboratory for Pesticide Residue Detection, Hangzhou, China; Department of Pesticide Science, College of Plant Protection, Nanjing Agricultural University; Jiangsu Key Laboratory of Pesticide Science, Nanjing, China.
Abstract:An efficient and sensitive enantioselective method for simultaneous determination of three acylamino acid fungicides in vegetables and fruits was presented by high-performance liquid chromatography (HPLC) coupled with tandem mass spectrometry. The three fungicides (benalaxyl, furalaxyl, and metalaxyl) residues in samples were extracted with acetonitrile containing 1% acetic acid and an aliquot was cleaned up with Si-(CH(2) )(3) -NH-(CH(2) )(2) -NH(2) and C(18) sorbent. Complete enantioseparation of three acylamino acid fungicides enantiomers was obtained under reversed-phase conditions on a cellulose tris (4-chloro-3-methylphenylcarbamate) column at 25°C using acetonitrile-0.1% formic acid solution (45:55, v/v) as a mobile phase. The elution orders of the eluted enantiomers were determined by a circular dichroism (CD) detector. The linearity, matrix effect, recovery, and precision were evaluated. Good linearity was obtained over the concentration range of 0.5-250 μg/L for each enantiomer in the standard solution and sample matrix calibration curves. There was no significant matrix effect for three fungicides determination based on the method. The inter-day mean recoveries, intra-day repeatability, and inter-day reproducibility varied from 81.3 to 95.7%, 2.2 to 9.4%, and 2.3 to 9.6%, respectively. The method provided high selectivity and sensitivity, and limits of quantification for enantiomers of three fungicides in vegetables and fruits were both 1 μg/kg.
Keywords:Benalaxyl  Enantioselective analysis  Furalaxyl  HPLC‐MS/MS  Metalaxyl
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