水产品中硝基呋喃代谢物残留快速检测新方法的研究

A Research to Establish a New Quick Determination of Nitrofuran Metabolite Residues in Aquatic Products

采用超高效液相色谱-串联质谱检测系统(UPLC-MS/MS)研究了2种衍生剂、2种衍生时间对水产品中4种硝基呋喃代谢物3-氨基-2-唑烷基酮(AOZ)、5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)、氨基脲(SEM)、1-氨基-乙丙酰脲(AHD)的衍生化反应机理、衍生产物的检测灵敏度及其稳定性。质谱扫描结果表明,衍生剂2-氯苯甲醛和2-硝基苯甲醛对4种硝基呋喃代谢物的衍生化反应遵循相同的亲核加成反应机理;方差分析结果表明,同一衍生剂和同一代谢物,快速衍生化2 h和连续衍生化16 h获得的衍生产物的检测灵敏度没有显著差别;所有快速衍生物检测灵敏度连续4 d保持相对稳定。初步研究了快速水解对阳性样品的有效性。

The derivatization mechanisms,the sensitivities and stabilities of the derivatives of 4 nitrofuran metabolites derivatised with 2 reagents,2-chlorobenzaldehyde and 2-nitrobenzaldehyde,with derivatisation time of 2 and 16 hours were studied,respectively,by a UPLC-MS/MS system to develop a quick analytical method for aquatic products.MS and MS-MS data indicated that both derivatization reactions with 2-chlorobenzaldehyde and 2-nitrobenzaldehyde involved a nucleophilic addition reaction.Mean square analysis showed there were no evident differences in sensitivities between derivatisation for 2 hours and for 16 hours given the same derivatisation reagent and the same metabolite,while sensitivities of all the quick derivatisations were relatively stable within 4 days.A premilinary research of the validity of rapid hydrolysis on the release of AOZ and SEM from inccurred samples was also carried out.