高效液相色谱/串联质谱法测定奶粉中的硝基呋喃代谢物  

Determination of Nitrofuran Metabolites in Milk Powder by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：彭涛[1] 储晓刚[2] 杨强[2] 李刚[2] 李建中[2] 李重九[1] 

机构地区：[1]中国农业大学理学院,北京100094 [2]中国检验检疫科学研究院,北京100025

出　　处：《分析化学》2005年第8期1073-1076,共4页Chinese Journal of Analytical Chemistry

基　　金：国家"十五"重大科技专项资助项目(No.2001BA804A18)

摘　　要：用高效液相色谱/串联质谱(LC-MS/MS)法同时测定奶粉中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的代谢物.盐酸水解奶粉中蛋白结合的代谢物,同时加入2-硝基苯甲醛(2-NBA),37℃过夜衍生化.加入硫酸锌,调pH值至7.0后,再加入亚铁氰化钾去除蛋白.后用乙酸乙酯提取,正己烷净化,分析物采用电喷雾电离正离子(ESI+)、多反应监测(MRM)模式检测,内标法定量.在添加浓度0.5～2 μg/kg范围内,内标法回收率为89.5%～110.3%;相对标准偏差(RSD)小于11.3%.5-马啉代甲基-3-氨基-2-恶唑酮(5-methylmorpholino-3-amino-2-oxazolidinone, AMOZ)、3-氨基-2-恶唑酮(3-amino-2-oxazolidinone, AOZ)方法检出限为0.05 μg/kg,氨基脲(semicarbazide, SEM)、1-氨基-乙内酰胺(1-amino-hydantoin, AHD)为0.1 μg/kg.A high performance liquid chromatography-tandem mass spectrometric method was established for simultaneous determination of the nitrofuran metabolites, furazolidone, furaltadone, nitrofurazone and nitrofurantoin in milk powder. Protein-bound metabolites were released in HCl solution and derivatised with 2-nitrobenzaldehyde （2-NBA） overnight at 37℃. Proteins were sedimentated by ZnSO4 and K4Fe （CN）6,after adjusting pH to 7.0. Then the analytes were extracted by ethyl acetate and cleaned up by n-hexane.Identification was achieved by electrospray ionization in positive mode （ESI^＋） using multiple reaction monitoring （MRM）. The quantification was performed with internal standards. The recoveries of 5-methylmorpholino-3-amino-2-oxazolidinone （ AMOZ ） , 3-amino-2-oxazolidinone （ AOZ ） , semicarbazide （ SEM ） and 1-amino-hydantoin （AHD） were in the range of 89.5% - 110.3% with spiked levels of 0.5 -2μg/kg. The RSDs were less than 11.3%. The limits of detection were 0.05μg/kg for AMOZ and AOZ, and 0.1 μg/kgfor SEM and AHD.

关 键 词：高效液相色谱 串联质谱法 测定 奶粉 硝基呋喃代谢物 药物残留 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]