色谱

色谱

• 研究报告 • 上一篇    下一篇

固相微萃取-高效液相色谱-荧光检测法测定番茄中的多菌灵和噻菌灵

胡彦学1,杨秀敏1,王志2,王春2,赵锦1

  

  1. 1. College of Food Science and Technology, Agricultural University of Hebei, Baoding 071001, China;
    2. College of Science, Agricultural University of Hebei, Baoding 071001, China
  • 收稿日期:2005-07-08 修回日期:1900-01-01 出版日期:2005-11-30 发布日期:1987-12-25
  • 通讯作者: 王志

Determination of Carbendazim and Thiabendazole in Tomatoes by Solid-Phase Microextraction Coupled with High Performance Liquid Chromatography and Fluorescence Detection

HU Yanxue1, YANG Xiumin1, WANG Zhi2, WANG Chun2, ZHAO Jin1   

  1. 1. College of Food Science and Technology, Agricultural University of Hebei, Baoding 071001, China;
    2. College of Science, Agricultural University of Hebei, Baoding 071001, China
  • Received:2005-07-08 Revised:1900-01-01 Online:2005-11-30 Published:1987-12-25

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摘要：

建立了应用固相微萃取(SPME)-高效液相色谱(HPLC)-荧光检测法测定番茄中多菌灵(MBC)和噻菌灵(TBZ)的分析方法。考察了萃取纤维、萃取时间、萃取温度、解吸时间、解吸液组成、解吸模式、pH值、有机溶剂和离子强度对MBC和TBZ萃取效率的影响，对SPME条件和色谱条件进行了优化。SPME在室温下进行,采用65 μm聚二甲基硅氧烷/二乙烯苯（PDMS/DVB）萃取纤维,萃取溶液中加入100 g/L NaCl,搅拌速度为1100 r/min,萃取时间为50 min。将该法用于番茄中MBC和TBZ的测定,MBC和TBZ的定量线性范围均为0.01~1.0 mg/kg;线性相关系数分别为0.9958和0.9967；检出限分别为0.003和0.001 mg/kg;回收率分别为83.5%和85.6%(n=5)，相对标准偏差(RSDs)分别为6.5%和3.8%。该方法操作简单,无需使用有机溶剂,适于分析番茄样品中的MBC和TBZ。

关键词: 多菌灵, 番茄 , 高效液相色谱, 固相微萃取, 噻菌灵, 荧光检测

Abstract:

A novel method for the determination of carbendazim (MBC) and thiabendazole (TBZ) in tomatoes by solid-phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) and fluorescence detection was developed. The experimental conditions of SPME, including extraction fiber, extraction time, extraction temperature, desorption time, desorption solvent, desorption mode, pH value, organic solvent and ionic strength, and HPLC conditions were optimized. The SPME for MBC and TBZ was performed on a 65 μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 50 min at room temperature with the solution being stirred at 1100 r/min. The florescence detection was made at 315 nm with excitation wavelength at 280 nm. The method is linear for MBC and TBZ over the range assayed from 0.01 to 1.0 mg/kg tomatoes with the detection limits of 0.003 mg/kg and 0.001 mg/kg and the correlation coefficients of 0.9958 and 0.9967, respectively. The average recoveries for MBC and TBZ were 83.5% and 85.6% with the relative standard deviations (RSDs) of 6.5% and 3.8%, respectively. The method is fast, simple, sensitive, solvent-free and suitable for the determination of MBC and TBZ in tomatoes.

Key words: fluorescence detection； carbendazim, high performance liquid chromatography, thiabendazole, tomatoes , solid-phase microextraction