多种提取手段联合液相色谱串联质谱法快速测定食品中苯霜灵残留量  

Quick Determination of Benalaxyl Residues in Foodstuffs by Multi-extraction Mode Combined HPLC-MS/MS

作　　者：祝伟霞 袁萍 杨冀州 王彩娟[2] 孙转莲 张巨洲 

机构地区：[1]河南出入境检验检疫局,河南郑州450003 [2]郑州大学化学系,河南郑州450042

出　　处：《现代食品科技》2012年第7期867-870,共4页Modern Food Science and Technology

基　　金：河南省科技攻关项目(122102110167);国家质检总局科研项目(2007IK162)

摘　　要：建立了高效液相色谱-电喷雾四极杆质谱技术测定13种食品中苯霜灵的确证方法。根据每种基质的特性,动物源性食品采用丙酮-正己烷提取,植物源性食品用乙酸乙酯提取,经石墨化碳与氨基(Carbon NH2)混合固相萃取柱净化,以乙腈-0.1%甲酸溶液为流动相,改性Shiseido MGⅡC18色谱柱中分离,电喷雾正离子多反应监测模式下监测。方法定量限(LOQ,S/N≥10)为5μg/kg,在2～100μg/L范围内呈良好的线性关系;13种食品基质添加三个浓度水平进行实验,加标平均回收率在66.0～104.2%之间,相对标准偏差为4.4%～12.3%。经验证本方法准确、快速,适合多种食品中苯霜灵残留的确证分析。A high performance liquid chromatography tandem quadrupole mass spectrum （LC-MS/MS） method was developed for confirmatively determining of benalaxyl residues in 13 foodstuffs. The benalaxyl was extracted with acetone-hexane in animal-origin foods and ethyl acetate in plant derived food. The purification was used with Carbon-NH2 solid-phase extraction （SPE） column. A mixture of acetonitrile and 0.1% formic acid was selected as the mobile phase and the separation was carded out on Shiseido MG Ⅱ C 18 column. The compound was analyzed quantitatively by mass spectrometry under positive electrospray ionization （ESI＋） multiple reaction monitoring （MRM） mode. The linear range of analyte was from 2 μtg/L to 100 μg/L and the limit of quantification （LOQ S/N≥10） was 5 μg/kg. Spiked with three concentration levels in 13 matrices, the method recoveries were between 66.0% and 104.2% with relative standard deviations 4.4% to 12.3%. The validated method was accurate, rapid and suitable for qualitatively determining benalaxyl residues in many foodstuffs.

关 键 词：液相色谱-串联质谱 苯霜灵 食品 残留测定 

分 类 号：TS207.53[轻工技术与工程—食品科学]