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采用反相分散固相萃取-超高效液相色谱-串联质谱法,利用多壁碳纳米管同时对植物源食品中两种新型异丙醇-三唑类杀菌剂进行对映体选择性测定。

Simultaneous Enantioselective Determination of Two New Isopropanol-Triazole Fungicides in Plant-Origin Foods Using Multiwalled Carbon Nanotubes in Reversed-Dispersive Solid-Phase Extraction and Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

Citrus Research Institute, Southwest University & Chinese Academy of Agricultural Sciences, Chongqing 400712, People's Republic of China.

Laboratory of Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture, Chongqing 400712, People's Republic of China.

出版信息

J Agric Food Chem. 2020 May 27;68(21):5969-5979. doi: 10.1021/acs.jafc.0c01385. Epub 2020 May 12.

DOI:10.1021/acs.jafc.0c01385
PMID:32347725
Abstract

A simple and sensitive enantiomeric analytical method was established for the determination of two new isopropanol-triazole fungicides mefentrifluconazole and ipfentrifluconazole in plant-origin foods using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The best enantioseparation of the four target stereoisomers was achieved on a Chiral MX(2)-RH column within 7 min by reversed-phase liquid chromatography, which is a significant improvement in the resolution of different chiral compounds under one set of conditions. A simple and effective pretreatment procedure was developed for the extraction and purification of the two target chiral fungicides using reversed-dispersive solid-phase extraction (r-DSPE) with multiwalled carbon nanotubes (MWCNTs). The influence of the type and amount of MWCNTs on the purification efficiencies and recoveries was evaluated. The mean recoveries for all four stereoisomers were in the range of 76.9-91.2%, with relative standard deviation (RSD) values below 7.2%. The limit of quantification (LOQ) of all stereoisomers of mefentrifluconazole and ipfentrifluconazole was 5 μg/kg for all tested matrixes. The results of the method validation and real samples analysis confirm that the established method is efficient and reliable for the enantiomeric determination of mefentrifluconazole and ipfentrifluconazole in plant-origin food samples.

摘要

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法,用于测定植物源食品中两种新型异丙醇三唑类杀菌剂甲呋氟菌唑和异丙定三唑的对映异构体。在反相液相色谱中,通过手性 MX(2)-RH 柱在 7 分钟内实现了四个目标立体异构体的最佳对映体分离,这是在一组条件下不同手性化合物分辨率的显著提高。采用多壁碳纳米管(MWCNTs)的反分散固相萃取(r-DSPE)建立了一种简单有效的预处理方法,用于两种目标手性杀菌剂的提取和纯化。评价了 MWCNTs 的类型和用量对净化效率和回收率的影响。所有四种立体异构体的平均回收率在 76.9-91.2%范围内,相对标准偏差(RSD)值低于 7.2%。所有测试基质中甲呋氟菌唑和异丙定三唑所有立体异构体的定量限(LOQ)均为 5μg/kg。方法验证和实际样品分析的结果证实,该方法可有效可靠地用于植物源食品样品中甲呋氟菌唑和异丙定三唑的对映体测定。

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