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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

[Determination of carbendazim and thiabendazole in tomatoes by solid-phase microextraction coupled with high performance liquid chromatography and fluorescence detection].

作者信息

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

机构信息

College of Food Science and Technology, Agricultural University of Hebei, Baoding 071001, China.

出版信息

Se Pu. 2005 Nov;23(6):581-4.

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 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 50 min at room temperature with the solution being stirred at 1 100 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 0.995 8 and 0.996 7, 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.

摘要

建立了一种基于固相微萃取(SPME)结合高效液相色谱(HPLC)和荧光检测法测定番茄中多菌灵(MBC)和噻菌灵(TBZ)的新方法。对SPME的实验条件进行了优化,包括萃取纤维、萃取时间、萃取温度、解吸时间、解吸溶剂、解吸方式、pH值、有机溶剂和离子强度,同时也优化了HPLC条件。采用65μm聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)纤维在室温下以1100r/min的转速搅拌溶液50min对MBC和TBZ进行SPME。荧光检测在315nm处进行,激发波长为280nm。该方法在0.01至1.0mg/kg番茄的测定范围内对MBC和TBZ呈线性,检测限分别为0.003mg/kg和0.001mg/kg,相关系数分别为0.9958和0.9967。MBC和TBZ的平均回收率分别为83.5%和85.6%,相对标准偏差(RSD)分别为6.5%和3.8%。该方法快速、简便、灵敏、无需使用溶剂,适用于番茄中MBC和TBZ的测定。

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