高效液相色谱-紫外检测法同时测定蜂蜜样品中的硝基咪唑残留量。

Simultaneous determination of nitroimidazole residues in honey samples by high-performance liquid chromatography with ultraviolet detection.

作者信息

Zhou Jinhui, Shen Jianzhong, Xue Xiaofeng, Zhao Jing, Li Yi, Zhang Jinzhen, Zhang Suxia

机构信息

Ministry of Agriculture, Chinese Academy of Agricultural Sciences, Apiculture Research Institute, Beeproduct Quality Supervision and Testing Center, Beijing 100093, People's Republic of China.

出版信息

J AOAC Int. 2007 May-Jun;90(3):872-8.

PMID:17580642

Abstract

A rapid and sensitive high-performance liquid chromatography (LC) method was developed for the simultaneous determination of metronidazole (MNZ), dimetridazole (DMZ), ronidazole (RNZ), tinidazole (TNZ), and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI) in honey. After extraction with ethyl acetate and evaporation, the residue containing the nitroimidazoles was dissolved in ethyl acetate-hexane and subjected to solid-phase extraction cleanup by amine extraction columns. The effluent was evaporated to dryness, and residues were dissolved and determined by LC with an ultraviolet detector set at 315 nm. The limits of detection were 1.0-2.0 ng/g for MNZ, DMZ, RNZ, TNZ, and HMMNI in honey. Average recoveries ranged from 71.5-101.4% in honey fortified at 10, 20, 50, and 100 ng/g. The method was validated for the analysis of real honey samples.

摘要

建立了一种快速灵敏的高效液相色谱（LC）方法，用于同时测定蜂蜜中的甲硝唑（MNZ）、二甲硝唑（DMZ）、洛硝哒唑（RNZ）、替硝唑（TNZ）和2-羟甲基-1-甲基-5-硝基咪唑（HMMNI）。用乙酸乙酯萃取并蒸发后，将含有硝基咪唑的残留物溶于乙酸乙酯-己烷中，并用胺萃取柱进行固相萃取净化。流出物蒸发至干，残留物溶解后用紫外检测器在315 nm波长下进行LC测定。蜂蜜中MNZ、DMZ、RNZ、TNZ和HMMNI的检测限为1.0 - 2.0 ng/g。在添加浓度为10、20、50和100 ng/g的蜂蜜中，平均回收率为71.5% - 101.4%。该方法经验证可用于实际蜂蜜样品的分析。