固相微萃取-高效液相色谱荧光检测法测定苹果中多菌灵和噻菌灵的灵敏方法

A sensitive determination method for carbendazim and thiabendazole in apples by solid-phase microextraction-high performance liquid chromatography with fluorescence detection.

作者信息

Hu Yanxue, Yang Xiumin, Wang Chun, Zhao Jin, Li Weining, Wang Zhi

机构信息

Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural University of Hebei, Baoding 071001, China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2008 Mar;25(3):314-9. doi: 10.1080/02652030701581864.

DOI:10.1080/02652030701581864

PMID:18311622

Abstract

A new analytical method for the determination of carbendazim (MBC) and thiabendazole (TBZ) in apples is reported, based on solid-phase microextraction (SPME) coupling HPLC with fluorescence detection. The main SPME and HPLC experimental conditions were optimized. The apples were first blended and centrifuged. Then, an aliquot of the resulting solution was subjected to SPME on a 60 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 35 min at room temperature with the solution being stirred at 1100 rev min(-1). The extracted pesticides on the SPME fibre were desorbed in the mobile phase into the SPME/HPLC interface for HPLC analysis. The method was linear over the range 0.01-1 mg kg(-1) in apples for both MBC and TBZ, with detection limits of 0.005 and 0.003 mg kg(-1) and correlation coefficients of 0.9995 and 0.9998, respectively. The average recoveries for MBC and TBZ were 91.5 and 92.3% with the relative standard deviations (RSD) of 4.7 and 4.1% at the 0.1 mg kg(-1) level, and 94.6 and 96.1% with RSD of 3.3 and 3.8% at the 0.5 mg kg(-1) level, respectively. The method is simple, sensitive, organic solvent-free and is suitable for the determination of MBC and TBZ in apples.

摘要

报道了一种基于固相微萃取（SPME）与高效液相色谱（HPLC）联用荧光检测法测定苹果中多菌灵（MBC）和噻菌灵（TBZ）的新分析方法。对主要的SPME和HPLC实验条件进行了优化。首先将苹果匀浆并离心。然后，取所得溶液的一份 aliquots 在 60 微米聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）纤维上于室温下进行 SPME 35 分钟，溶液以 1100 转/分钟（-1）搅拌。SPME 纤维上萃取的农药在流动相中解吸进入 SPME/HPLC 接口进行 HPLC 分析。该方法在苹果中 MBC 和 TBZ 的含量范围为 0.01 - 1 毫克/千克时呈线性，检测限分别为 0.005 和 0.003 毫克/千克，相关系数分别为 0.9995 和 0.9998。在 0.1 毫克/千克水平下，MBC 和 TBZ 的平均回收率分别为 91.5%和 92.3%，相对标准偏差（RSD）分别为 4.7%和 4.1%；在 0.5 毫克/千克水平下，平均回收率分别为 94.6%和 96.1%，RSD 分别为 3.3%和 3.8%。该方法简单、灵敏、无需有机溶剂，适用于苹果中 MBC 和 TBZ 的测定。