高效液相色谱-串联质谱法快速测定6类食品中增效醚的残留  

Rapid determination of piperonyl butoxide residues in 6 kinds foodstuffs with high performance liquid chromatography tandem mass spectrometry

作　　者：祝伟霞 杨冀州 刘朝晖 袁萍 王彩娟[2] 张巨洲 孙转莲 

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

出　　处：《分析试验室》2012年第9期77-80,共4页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科研项目(2007IK162);行业标准修订项目(2008B262r)资助

摘　　要：建立了水果、蔬菜、粮谷、油料、动植物脂类、动物源性食品等6类食品中增效醚残留量快速测定的液相色谱-质谱/质谱(LC-MS/MS)方法。样品盐析并除水后,用三氯甲烷提取,氟罗里硅土填料固相萃取柱净化,丙酮-三氯甲烷混合溶剂洗脱,以乙腈-0.1%甲酸为流动相,在Zobax SB C18液相色谱柱完成分离,并于电喷雾正离子多反应监测模式下质谱测定。考察了提取溶剂、净化方法、柱容量、仪器条件、基质效应对分析结果的影响。增效醚质量浓度在0.5～100μg/L范围内,线性相关系数(r)为0.9976,方法定量限(LOQ)为10μg/kg。17种食品基质添加LOQ、低MRL、2倍MRL、高MRL 4个不同浓度水平时,回收率在80.3%～96.3%之间,相对标准偏差为2.7%～14%,方法可以满足多种食品基质中增效醚残留量的定性和定量检测要求。A rapid confirmative method was developed for the determination of piperonyl butoxide residues in 6 kinds of foodstuffs, such as fruits, vegetables, cereals, oilseeds, animal and vegetable oils, animal-origin foods by liquid chromatography tandem mass spectrometry （LC-MS/MS）. After sahed-out and removed-water, the sample was extracted with chloroform, then clean-up procedure was selected with florisil solid-phase extraction （SPE） and the analyte were eluted with acetone-chloroform solvent. The separation was performed on a Zobax SB Cl8 column with the mobile phase of acetonitrile-0. 1% formic acid. The piperonyl butoxide was analyzed quantitatively by mass spectrometry with positive electrospray ionization （ESI ＋ ） multiple reaction monitoring （MRM） mode. The influence factors including extraction, purification, column capacity, chromatographic or mass spectrometric conditions, and matrix effects were optimized. With the linearity in the range of 0.5 - 100 p,g/L, the obtained r value was 0. 9976. The limit of quantification was 10 p,g/kg. The method recoveries varied from 80. 3% to 96. 3% and the relative standard deviations （RSD） were between 2. 7% and 14%. The validated method was simple, fast, sensitive, and was satisfactory with requirements of detection of piperonyl butoxide residues in various food matrices.

关 键 词：增效醚 液相-质谱/质谱 固相萃取 食品 残留 

分 类 号：O657.63[理学—分析化学]