School of Pharmacy , Shenyang Pharmaceutical University , Shenyang 110016 , China.
Daicel Chiral Technologies (China) Co., Ltd , Shanghai 200131 , China.
J Agric Food Chem. 2019 Aug 21;67(33):9362-9370. doi: 10.1021/acs.jafc.9b01850. Epub 2019 Aug 12.
This manuscript presents an effective and robust method for simultaneous stereoselective determination of two pyrethroid insecticides, tetramethrin and α-cypermethrin in different food products by high-performance liquid chromatography. Enantioseparation was carried out using reversed-phase chromatography, and the influences of four polysaccharide-based chiral columns, mobile phase composition, and column temperature on retention were fully investigated. Satisfactory separation was obtained on Chiralpak IG column using acetonitrile-water (75:25, v/v) under isocratic conditions. To extract and purify the target analytes from food matrices, matrix solid-phase dispersion was employed with C as dispersant and primary secondary amine as well as graphitized carbon black as cleanup sorbents. Response surface method based on Box-Behnken design was implemented to assist optimization of the extraction variables. Then, method validation was done in real samples including specificity, linearity, sensitivity, trueness, precision, as well as stability, and its analytical performance fulfills the criteria recommended by the European Union SANTE/11945/2015, demonstrating its applicability in studying the stereochemistry of chiral tetramethrin and α-cypermethrin in food products.
本文提出了一种高效、稳健的方法，通过高效液相色谱法同时立体选择性测定不同食品中两种拟除虫菊酯杀虫剂，四氟甲醚菊酯和α-氯氰菊酯。手性分离采用反相色谱法，充分考察了四种多糖基手性柱、流动相组成和柱温对保留的影响。在 Chiralpak IG 柱上，以乙腈-水（75:25，v/v）为流动相，在等度条件下可获得满意的分离。为了从食品基质中提取和纯化目标分析物，采用基质固相分散法，以 C 为分散剂，仲胺和石墨化炭黑为净化吸附剂。基于 Box-Behnken 设计的响应面法用于辅助提取变量的优化。然后，在实际样品中进行了方法验证，包括特异性、线性、灵敏度、准确度、精密度以及稳定性，其分析性能符合欧盟 SANTE/11945/2015 推荐的标准，证明了其在手性四氟甲醚菊酯和α-氯氰菊酯在食品中立体化学研究中的适用性。
