Enantiomeric Resolution of Chiral Pesticides by High-Performance Liquid Chromatography

Peng Wang,† Shuren Jiang,† Donghui Liu,† Hongjun Zhang,‡ and Zhiqiang Zhou*†
Department of Applied Chemistry, China Agricultural University, Beijing 100094, and Institute for Control of Agrochemicals Ministry of Agriculture, Beijing 100026, China
J. Agric. Food Chem., 2006, 54 (5), pp 1577–1583
DOI: 10.1021/jf052631o
Publication Date (Web): February 11, 2006
Copyright © 2006 American Chemical Society
†

 China Agricultural University.

,
‡

 Institute for Control of Agrochemicals Ministry of Agriculture.

,
*

 To whom correspondence should be addressed. Tel:  (086)010-62731294. Fax:  (086)010-62732937. E-mail:  zqzhou@cau.edu.cn.

Abstract

Successful enantiomeric separation of 10 chiral pesticides by high-performance liquid chromatography (HPLC) using cellulose-tris(3,5-dimethylphenylcarbamate) (CDMPC) chiral stationary phase (CSP) was performed. The mobile phase was n-hexane modified by ethanol, propanol, 2-propanol (IPA), butanol, or isobutanol. The effects of mobile phase composition and column temperature on the separation were investigated. Baseline separation was obtained with ethofumesate, fluroxypyr-meptyl, malathion, benalaxyl, diclofop-methyl, methamidophos, vinclozolin, and lactofen, whereas near baseline separation was obtained with profenofos and acetochlor. Butanol was the best modifier for benalaxyl; isobutanol was the best modifier for lactofen, malathion, diclofop-methyl, and ethofumesate; and IPA was the best modifier for the other five. Better separations were not always at low temperature. The elution orders of the eluting enantiomers were determined by a circular dichroism (CD) detector. The quantitative analysis methods for the enantiomers of ethofumesate, benalaxyl, and diclofop-methyl were established. Validation parameters include linearity, precision, and limit of detection (LOD). The enantiomeric residual analysis procedures in soil and water samples were also developed using acetone extraction and C18 solid phase extraction. The methods were reliable for residual analysis of the enantiomers.

Keywords: Enantiomeric resolution; HPLC; chiral pesticides

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History

  • Published In Issue March 08, 2006
  • Received for review October 24, 2005. Revised manuscript received January 15, 2006. Accepted January 19, 2006. This work was supported by National Natural Science Foundation of China (20377052).

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