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Enantioselective determination of acylamino acid fungicides in vegetables and fruits by chiral liquid chromatography coupled with tandem mass spectrometry
Author(s) -
Zhang Hu,
Wang Xinquan,
Jin Lixia,
Qian Mingrong,
Wang Xiangyun,
Xu Hao,
Qi Peipei,
Wang Qiang,
Wang Minghua
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200063
Subject(s) - chemistry , chromatography , tandem mass spectrometry , enantiomer , formic acid , elution , repeatability , high performance liquid chromatography , mass spectrometry , organic chemistry
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.