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几种有机磷农药在固定化多糖手性固定相上的分离。

The separation of several organophosphate pesticides on immobilized polysaccharide chiral stationary phases.

机构信息

Senior Method Development Chemist, WLC, WLW, Champion, Watts Technology and Method Development Chiral Technologies, Inc, West Chester, Pennsylvania, USA.

Technology and Business Development Manager, WJU, Umstead Technology and Method Development Chiral Technologies, Inc, West Chester, Pennsylvania, USA.

出版信息

Chirality. 2022 Aug;34(8):1078-1093. doi: 10.1002/chir.23473. Epub 2022 May 31.

Abstract

While not initially a focus or priority, in recent decades, an emphasis has been placed on the activity of individual enantiomers of widely used pesticides. Of particular note are organophosphorus-based pesticides like fenamiphos and profenofos, as examples. This work explores the enantioselective high-performance liquid chromatography (HPLC) separations of seven such organophosphorus pesticides (OP's) on the library of immobilized polysaccharide-based chiral stationary phases (CSPs) with normal phase hexane/alcohol mixtures. Further exploration of the effect of mobile phase strength and temperature on several of the separations was performed using simple factorial design. Equivalent retention of the first eluting enantiomer of several combinations of temperature and mobile phase was compared for peak shape, selectivity, and resolution. Similarly, equivalent selectivity of several combinations of temperature and mobile phase was compared for peak shape, retention of the first eluting enantiomer, and resolution. The results of this study make available several new chiral separations of the OPs included in the work that were not previously documented, including separations on the three most recently commercialized phases, Chiralpak IH, IJ, and IK. Additionally, sufficient understanding was obtained to be able to predict the trade-off of resolution, analysis time, peak sharpness (and thus improve limit-of-detection [LOD]/limit-of-quantification [LOQ]), robustness, and convenience of conditions for further application optimization.

摘要

虽然最初不是重点或优先事项,但近几十年来,人们越来越关注广泛使用的农药的单个对映异构体的活性。以有机磷杀虫剂如 fenamiphos 和 profenofos 为例,这方面的工作尤其值得注意。本研究探索了七种有机磷农药 (OP) 在固定化多糖手性固定相 (CSP) 库上的对映选择性高效液相色谱 (HPLC) 分离,使用正相己烷/醇混合物作为流动相。使用简单的因子设计进一步研究了流动相强度和温度对几种分离的影响。比较了几种温度和流动相组合的第一个出峰对映异构体的等效保留时间,以比较峰形、选择性和分辨率。同样,比较了几种温度和流动相组合的等效选择性,以比较峰形、第一个出峰对映异构体的保留时间和分辨率。本研究的结果提供了几种以前未记录的 OP 的新手性分离,包括在最近商业化的三个阶段,Chiralpak IH、IJ 和 IK 上的分离。此外,还获得了足够的理解,能够预测分辨率、分析时间、峰形尖锐度(从而提高检测限[LOD]/定量限[LOQ])、稳健性和条件便利性之间的权衡,以进一步优化应用。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/541a/9544164/6007fa28e003/CHIR-34-1078-g011.jpg

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