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.
出处
《现代食品科技》
EI
CAS
北大核心
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)
