Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

被引：57

作者：

Xia, Xi ^{[1
]}

Ding, Shuangyang ^{[1
]}

Li, Xiaowei ^{[1
]}

Gong, Xiao ^{[1
]}

Zhang, Suxia ^{[1
]}

Jiang, Haiyang ^{[1
]}

Li, Jiancheng ^{[1
]}

Shen, Jianzhong ^{[1
]}

机构：

[1] China Agr Univ, Coll Vet Med, Dept Pharmacol & Toxicol, Beijing 100193, Peoples R China

来源：

ANALYTICA CHIMICA ACTA | 2009年 / 651卷 / 02期

关键词：

Melamine; Gas chromatography; Ultra-performance liquid chromatography; Mass spectrometry; Egg; METABOLITE MELAMINE; CYROMAZINE; PRODUCTS; RESIDUES; TISSUE; FOOD;

D O I：

10.1016/j.aca.2009.08.025

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (CC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 mu g kg(-1), respectively. This validated method was successfully applied to the determination of melamine in real samples from market. (C) 2009 Elsevier B.V. All rights reserved.

引用

页码：196 / 200

页数：5