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手性分离和反相高效液相色谱法测定蔬菜中乙唑螨腈对映体。

Chiral Separation and Determination of Etoxazole Enantiomers in Vegetables by Normal-Phase and Reverse-Phase High Performance Liquid Chromatography.

机构信息

Key Laboratory of Entomology and Pest Control Engineering, College of Plant Protection, Southwest University, Chongqing 400715, China.

Academy of Agricultural Sciences, Southwest University, Chongqing 400715, China.

出版信息

Molecules. 2020 Jul 9;25(14):3134. doi: 10.3390/molecules25143134.

DOI:10.3390/molecules25143134
PMID:32659902
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7397032/
Abstract

The chiral separation of etoxazole enantiomers on Lux Cellulose-1, Lux Cellulose-3, Chiralpak IC, and Chiralpak AD chiral columns was carefully investigated by normal-phase high performance liquid chromatography and reverse-phase high performance liquid chromatography (HPLC). Hexane/isopropanol, hexane/-butanol, methanol/water, and acetonitrile/water were used as mobile phase at a flow rate of 0.8 mL/min. The effects of chiral stationary phase, mobile phase component, mobile phase ratio, and temperature on etoxazole separation were also studied. Etoxazole enantiomers were baseline separated on Lux Cellulose-1, Chiralpak IC, and Chiralpak AD chiral columns, and partially separated on Lux Cellulose-3 chiral column under normal-phase HPLC. However, the complete separation on Lux Cellulose-1, Chiralpak IC, and partial separation on Chiralpak AD were obtained under reverse-phase HPLC. Normal-phase HPLC presented better resolution for etoxazole enantiomers than reverse-phase HPLC. Thermodynamic parameters, including Δ and Δ, were also calculated based on column temperature changes from 10 °C to 40 °C, and the maximum resolutions () were not always acquired at the lowest temperature. Furthermore, the optimized method was successfully applied to determine etoxazole enantiomers in cucumber, cabbage, tomato, and soil. The results of chiral separation efficiency of etoxazole enantiomers under normal-phase and reverse-phase HPLC were compared, and contribute to the comprehensive environmental risk assessment of etoxazole at the enantiomer level.

摘要

手性分离 Lux Cellulose-1、Lux Cellulose-3、Chiralpak IC 和 Chiralpak AD 手性柱上乙恶唑对映异构体通过正相高效液相色谱法和反相高效液相色谱法（HPLC）进行了仔细研究。正相 HPLC 中，以 0.8 mL/min 的流速使用正己烷/异丙醇、正己烷/-丁醇、甲醇/水和乙腈/水作为流动相；反相 HPLC 中，研究了手性固定相、流动相组成、流动相比例和温度对乙恶唑分离的影响。乙恶唑对映异构体在 Lux Cellulose-1、Chiralpak IC 和 Chiralpak AD 手性柱上基线分离，在 Lux Cellulose-3 手性柱上部分分离。然而，在反相 HPLC 下，乙恶唑对映异构体在 Lux Cellulose-1、Chiralpak IC 上完全分离，在 Chiralpak AD 上部分分离。正相 HPLC 对乙恶唑对映异构体的分辨率优于反相 HPLC。还基于柱温从 10°C 变化到 40°C 计算了热力学参数，包括Δ和Δ，而并非在最低温度下总是获得最大分辨率（）。此外，优化的方法成功应用于黄瓜、白菜、番茄和土壤中乙恶唑对映异构体的测定。比较了正相和反相 HPLC 下手性分离乙恶唑对映异构体的效率，有助于在对映体水平上对乙恶唑进行综合环境风险评估。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/74b558f53f9a/molecules-25-03134-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/0133fb257cd7/molecules-25-03134-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/ce29b49c6131/molecules-25-03134-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/a5334f991455/molecules-25-03134-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/74b558f53f9a/molecules-25-03134-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/0133fb257cd7/molecules-25-03134-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/ce29b49c6131/molecules-25-03134-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/a5334f991455/molecules-25-03134-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/449f/7397032/74b558f53f9a/molecules-25-03134-g004.jpg

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