液相色谱-串联质谱法测定液态乳制品中的苯代三聚氰胺  

Determination of Benzoquanmine in Liquid Products of Milk by LC-MS / MS

作　　者：郝成婷[1] 王红松 徐炎 周志荣 陈智栋[1] 

机构地区：[1]常州大学石油化工学院,江苏常州213022 [2]常州出入境检验检疫局,江苏常州213022

出　　处：《分析测试学报》2014年第2期227-230,共4页Journal of Instrumental Analysis

基　　金：国家质量监督检验检疫总局科技计划资助项目(2012IK207)

摘　　要：建立了液态乳制品中苯代三聚氰胺的高效液相色谱-串联质谱（HPLC-MS/MS）测定方法.优化了前处理条件、液相色谱和质谱参数.样品经LC-C18固相萃取柱富集净化后,采用ZORBAX Eclipse Plus C18色谱柱分离,流动相为乙腈-水（15∶85,体积比）,流速为0.3 mL/min.采用正离子模式的电喷雾质谱检测,多反应（MRM）选择离子监测,定量离子与定性离子分别为m/z 104.1与m/z 146.0,外标法定量.结果表明,苯代三聚氰胺在2～100 μg/L范围内线性关系良好,相关系数为0.9991,方法的检出限和定量下限分别为1.0 μg/kg和3.0 μg/kg.在低、中、高3个加标水平下的平均回收率为77％ ～ 105％,相对标准偏差（RSD）为2.3％ ～ 5.0％.该方法操作简单、准确可靠,适用于液态乳制品中苯代三聚氰胺的测定.A method was developed for the determination of benzoquanmine in liquid products of milk by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The conditions of extraction and parameters of LC-MS were optimized.The sample was enriched and pufffied with an LC-C18 SPE cartridge,then separated on a ZORBAX Eclipse Plus C18 column using a mixture of acetonitrile-water（15 ∶ 85） as mobile phase at a flow rate of 0.3 mL/min.The detection of benzoquanmine was performed by mass spectrometry（ESI-MS） under positive-ion electrospray ionization mode.The two precursor-product ion pairs,m/z 104.1 and m/z 146.0,were used as the quantitative and qualificative ions,respectively.The external standard method was used for quantitative analysis.The results showed that a good linearity for benzoquanmine existed in the range of 2-100 μg/L with a correlation coefficient of 0.999 1.The limits of detection（LODs） and limits of quantitation （LOQs） were 1.0 μg/kg and 3.0 μg/kg,respectively.The average recoveries of benzoquanmine at three spiked levels were in the range of 77%-105%,with relative standard deviations（RSDs） of 2.3%-5.0%.The proposed method was simple and accurate,and was suitable for the determination of benzoquanmine in liquid products of milk.

关 键 词：苯代三聚氰胺 液相色谱-串联质谱 乳制品 

分 类 号：O657.63[理学—分析化学] TQ042[理学—化学]