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超临界流体色谱-串联质谱法测定烟草及土壤中西玛津对映体

A green and effective method for the determination of metalaxyl enantiomers in tobacco and soil by supercritical fluid chromatography-tandem mass spectrometry.

机构信息

China National Tobacco Quality Supervision and Test Center, Zhengzhou, China.

Zhengzhou Tobacco Research Institute of CNTC, Zhengzhou, China.

出版信息

Chirality. 2020 May;32(5):505-514. doi: 10.1002/chir.23184. Epub 2020 Feb 21.

DOI:10.1002/chir.23184
PMID:32084304
Abstract

We reported a new methodology for the stereoselective determination of metalaxyl enantiomers in tobacco and soil. The QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used for the extraction and clean-up of the tobacco and soil samples. Separation of the metalaxyl enantiomers was performed on an ACQUITY UPC2 Trefoil CEL1 chiral column coupled with supercritical fluid chromatography with tandem mass spectrometry (SFC-MS/MS), and the run time was only 5 minutes. Under the optimized conditions, the recoveries for the enantiomers were between 78.2% and 93.3% with intraday relative standard deviations (RSDs) ranging from 1.1% to 5.4%. The limit of detection (LOD) for the enantiomers in tobacco and soil varied from 0.005 to 0.007 mg/kg, and the limit of quantitation (LOQ) ranged from 0.017 to 0.020 mg/kg. In this method, only a small amount of methanol was consumed to obtain a rapid stereoselective separation. This proposed method showed good accuracy and precision and might be suitable for fast enantioselective determination of metalaxyl in food and environmental samples. The developed method was further validated by application to the analysis of authentic samples.

摘要

我们报道了一种新的方法,用于立体选择性测定烟草和土壤中的金属砜。QuEChERS(快速、简单、廉价、有效、坚固、安全)方法用于提取和净化烟草和土壤样品。采用 ACQUITY UPC2 Trefoil CEL1 手性柱与超临界流体色谱-串联质谱(SFC-MS/MS)对金属砜对映异构体进行分离,运行时间仅为 5 分钟。在优化条件下,对映异构体的回收率在 78.2%至 93.3%之间,日内相对标准偏差(RSD)在 1.1%至 5.4%之间。对映异构体在烟草和土壤中的检出限(LOD)为 0.005 至 0.007mg/kg,定量限(LOQ)为 0.017 至 0.020mg/kg。在该方法中,仅消耗少量甲醇即可实现快速立体选择性分离。该方法具有良好的准确性和精密度,可能适用于食品和环境样品中金属砜的快速对映选择性测定。该方法通过应用于真实样品的分析进一步得到验证。

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