School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road Shenhe District, 110016, Shenyang, Liaoning Province, PR China.
Daicel Chiral Technologies (China) Co., Ltd, No.32, HeXiang Road, WaiGaoQiao Free Trade Zone, Shanghai, 200131, PR China.
J Pharm Biomed Anal. 2019 Oct 25;175:112784. doi: 10.1016/j.jpba.2019.112784. Epub 2019 Jul 21.
This work presented a novel method for the simultaneous enantioselective analysis of six chiral pesticides in seven functional foods at enantiomeric levels. Samples were extracted from matrices using a magnetic solid-phase extraction method based on FeO modified carbon nanospheres as adsorbent. Experimental variables were optimized using one-variable-at-a-time and response surface methodology. Six chiral pesticides were simultaneously enantio-separated under one chromatographic condition using Chiralpak IG column, and a reversed-phase liquid chromatography coupled with tandem mass spectrometry was used for their sensitive and selective quantification. Under the optimum conditions, good linearity was obtained for all enantiomers with correlation coefficients (R) greater than 0.9912. The mean recoveries of the analytes were in the range of 84.0-105.2%, with intra- and inter-batch precision less than 10.9% and 11.4%, respectively. Method quantification limits varied from 1 to 4 ng g in all the tested matrices. The developed method was successfully applied to real samples to monitor the occurrence and enantiomeric composition of chiral pesticides, demonstrating its applicability for the routine analysis of chiral pesticide residues in food samples.
本工作提出了一种新的方法,用于在七种功能食品中同时对六种手性农药进行对映体水平的分析。样品采用基于 FeO 修饰碳纳米球的磁性固相萃取方法从基质中提取。实验变量采用单变量法和响应面法进行优化。六种手性农药在一种色谱条件下使用 Chiralpak IG 柱同时进行对映体分离,并采用反相液相色谱-串联质谱法进行灵敏和选择性定量。在最佳条件下,所有对映体均具有良好的线性,相关系数(R)大于 0.9912。分析物的平均回收率在 84.0-105.2%之间,批内和批间精密度均小于 10.9%和 11.4%。在所有测试的基质中,方法的定量限范围为 1-4 ng g。该方法成功应用于实际样品,用于监测手性农药的发生和对映体组成,证明其在手性农药残留的常规分析中具有适用性。