亲水作用色谱-串联质谱测定蔬菜中灭蝇胺及其代谢物三聚氰胺  

Determination of Cyromazine and Melamine Residues in Vegetables by Triple Quadurupole Liquid Chromatography-Tandem Mass Spectrometry with Hydrophilic Interaction Chromatography

作　　者：钱鸣蓉[1] 章虎[1] 何红梅[1] 王祥云[1] 陈志民[1] 吴俐勤[1] 

机构地区：[1]浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《分析化学》2009年第6期902-906,共5页Chinese Journal of Analytical Chemistry

基　　金：浙江省重大科技攻关项目(No.2005C12007);杭州市科技发展计划(No.20080632B08)资助

摘　　要：建立了亲水作用色谱-串联质谱测定蔬菜中灭蝇胺及其代谢物三聚氰胺的方法。蔬菜样品匀浆后经甲醇-水提取,取适量酸化后提取液经阳离子固相萃取柱净化,洗脱液用氮气吹干,残留物用5 mL流动相定容。采用亲水作用色谱(Hilic)分离,在电喷雾-选择反应监测模式下,进行定性和定量分析。以基质校正曲线计算,添加浓度为0.04和0.20 mg/kg时,灭蝇胺的回收率为84.2%～101.3%;相对标准偏差(RSD)为4.5%～10.7%;三聚氰胺的回收率为72.5%～97.1%;RSD为4.3%～10.8%;灭蝇胺和三聚氰胺的定量限分别为0.01和0.005 mg/kg。利用本方法检测了多种蔬菜样品中灭蝇胺、三聚氰胺的含量。A fast, sensitive and specific method was developed to determine cyromazine and its metabolite melamine in vegetables. The targets were extracted with the mixture of methanol-water（9： 1, V/V） from vege- tables. The pH of extract was adjusted with hydrochloric acid. Then partial extract was purified through strong cation-exchange cartridge without concentration. After the residues were eluted with 8 mL methanol-ammonium solution（95：5, V/V）, the eluate was evaporated to dry with nitrogen stream and then dissolved in 5 mL mobile phase. Hydrophilie interaction chromatography combined with MS/MS was used to simultaneously determine eyromazine and melamine. The mobile phase was composed of acetonitrile and water with 0. 1% formic acid（9：1, V/V）. The correlation coefficient was 0. 999 for both compounds when concentrations ranged from O. 01 to 0.25 mg/L. Signals of cyromazine and melamine were suppressed in matrices. The peak area of cyromazine in matrices reduced to 41% -52%. And the peak area of melamine in matrices reduced to 78%. At fortification level of 0.04 and 0.20 mg/kg in vegetables, the average recoveries were 84.25% - 101.3% for cyromazine and 72.5% -97.1% for melamine. And the RSD was 4.5% -10.7% for cyromazine and 4. 3% - 10.8% for melamine. The LOD was 0.01 mg/kg for cyromazine and 0. 005 mg/kg for melamine. The method was used to determine the cyroInazine and melamine residues in vegetables from market.

关 键 词：蔬菜 灭蝇胺 三聚氰胺 亲水作用色谱 串联质谱 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程]