超临界流体色谱串联质谱法研究葡萄中乙虫腈对映体的选择性降解

Degradation Dynamics of Ethiprole Enantiomers in Grape by Supercritical Fluid Tandem Mass Spectrometry

为探索乙虫腈对映体在葡萄中的消解动态,利用超临界流体串联质谱(SFC-MS/MS)建立一种简单、灵敏、绿色的手性分析方法用于检测葡萄中的乙虫腈对映体。在负离子扫描喷雾下,使用OD-3手性柱,以二氧化碳/异丙醇(90/10,v/v)为流动相,柱温30℃,流速为1.8 mL·min^(-1),背压为2 000 psi时,乙虫腈对映体得到完全分离。采用改进的QuEChERS方法检测葡萄中乙虫腈对映体,该方法的平均回收率均为86.2%~111.6%,LOQ为10μg·kg^(-1)。结果表明:在葡萄中,R-(+)-乙虫腈优先降解,导致S-(-)-乙虫腈相对富集。研究结果可为评估乙虫腈对映体的环境风险提供支持。

A simple,sensitive and green method for the enantioselective determination of ehiprole enantiomers in grape had been established using supercritical fluid chromatography SFC-MS/MS for determind the degradation of ethiprole enantiomers in grape.The optimal SFC-MS/MS working conditions were determined to include a CO/IPA mobile phase(90:10,v/v),1.8 mL·min^(-1) flow rate,2 000 psi ABPR,and 30 ℃ column temperature using a Chiralpak OD-3 chiral column under electrospray ionization negative mode.The modified QuEChERS method was applied to grape samples.The mean recoveries for the ethiprole enantiomers were 86.2%11.6%.The LOQ of ethiprole enantiomer was 10.0 μg·kg^(-1).The results showed that R-(+)-ethiprole was preferentially degraded in grapes,resulting in relative enrichment of S-(-)-ethiprole.The results of this study are helpful to further evaluate the environmental risk of ethiprole enantiomers.