色谱2011，Vol.29Issue(7)：637-642,6.DOI:10.3724/SP.J.1123.2011.00637
高效液相色谱-串联质谱法测定食品中多杀菌素A和D的残留量
Determination of spinosyns A and D residues in food by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS ) method was established for the determination of spinosyns A and D residues in foodstuffs.The food samples were extracted with acetonitrile-water ( 50∶50 , V/V ), and then purified by an HLB solid phase extraction ( SPE ) column. The analytes were determined by HPLC-MS/MS and quantified by external standard method. The mass spectrometric detection was operated with electrospray in positive ionization mode and the spinosyns A and D were identified in multiple reaction monitoring ( MRM ) mode. The linear range of the method was 1 - 20 μg/L, with the correlation coefficient ( r2 ) of 0.9999. No significant matrix effect was found for spiked samples. The recoveries of spinosyns A and D spiked in food were 76.2％ - 114.0％ at the spiked levels of 1 - 10 μg/kg. The relative standard deviations ( RSDs ) were less than 10％. The limits of detection ( LODs ) and quantification ( LOQs ) were 0.2 μg/kg and 0.5 μg/kg for spinosyn A,0.5 μg/kg and 1.0 μg/kg for spinosyn D , respectively. The proposed procedure was applied to the analysis of 969 real samples from Xiamen, Fujian Province ( China ), of which 15 positive samples were found. The results showed that the proposed method is sensitive and accurate for the determination of spinosyns A and D in foodstuffs.关键词
高效液相色谱-串联质谱法/多杀菌素/多杀菌素A/多杀菌素D/食品Key words
high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS )/ spinosad/ spinosyn A/ spinosyn D/ food分类
化学化工引用本文复制引用
张缙,杨黎忠,林立毅,陈鹭平,周昱,徐敦明..高效液相色谱-串联质谱法测定食品中多杀菌素A和D的残留量[J].色谱,2011,29(7):637-642,6.基金项目
厦门市科技计划项目(3502Z20092009、3502Z20102012)和国家质检总局科技计划项目(2010IK192). （3502Z20092009、3502Z20102012）
