液相色谱-串联质谱法测定牛奶和奶粉中卡巴氧和喹乙醇代谢物的残留量  

Determination of the residues of metabolites of carbadox and olaquindox in milk and milk powder-LC-MS-MS method

作　　者：林黎[1] 谢丽琪[1] 欧阳姗[1] 梁宏[1] 叶刚[1] 廖菁菁[1] 庞国芳[2] 

机构地区：[1]深圳出入境检验检疫局,深圳518067 [2]秦皇岛出入境检验检疫局,秦皇岛066000

出　　处：《分析试验室》2010年第2期38-41,共4页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局制标(20079610-T-469)项目资助

摘　　要：建立了牛奶和奶粉中卡巴氧代谢物喹喔啉-2．羧酸（QCA）和喹乙醇代谢物3-甲基喹喔啉-2-总羧酸（MQCA）残留量的液相色谱-串联质谱测定方法。将样品经0．6％（体积分数）的甲酸溶液进行消化，用Tris缓冲溶液调节pH后，加入Protease蛋白酶进行酶解，样品溶液用0．3mol／LHCl溶液酸化后，采用阴离子交换固相萃取柱OasisMAX进行净化和富集。分析样品以0．1％（体积分数）的甲酸溶液-甲醇-乙腈为流动相，经Inertsil ODS-3色谱柱分离，采用负离子扫描，在LC．MS／MS多反应监测模式下进行定性及定量分析。喹吧啉-2-羧酸和3-甲基喹嘿啉-2-羧酸的方法测定下限牛奶为0．5μg／kg，奶粉为4．0μ/Kg。对牛奶在0．5～5．0μg／kg，奶粉在4．0～40．0μg/kg添加水平的平均回收率为68．2％～82．5％，RSD为3．4％～12％。This study presented a liquid chmmatography-tandam mass spectrometry （I_E-MS/MS） method for determi- nation of residues of Carbadox, Olaquindox and related metabolites quinoxalie-2-carboxylic acid（QCA） and 3-meth- ylquinoxaline-2-carboxylic acid （MQCA） in milk and milk powder. As for the extraction of QCA and MQCA, milk and milk powder is first digested with 0.6% formic acid to deactivate naturally-occurring enzymes. After overnight enzy- matic hydrolysis with protease, the tissue extract is acidified, centrifuged and filtered. QCA and MQCA are recovered from the tissue extract by using an Oasis MAX solid phase extraction （SPE） cartridge. The analytes are separated on a Inertsil ODS-3 LC column, and qualitatively and quantitatively determined under multi-reaction monitoring （MRM） scan type with tandem mass analyzer using positive polarity mode. The limit of quatitation （LOQ） for the two analytes in milk is 0.5 μg/kg, in milk power is 4.0 μg/kg. At the spiked level in the range of 0.5 - 5.0 μg/kg in milk and 4.0 - 40.0μg,/kg in milk power, the mean recoveries are in the range of 68.2% - 82.5%, the relative standard deviation are in the range of 3.4% - 12%.

关 键 词：液相色谱-串联质谱 卡巴氧 喹乙醇 代谢产物 牛奶 奶粉 

分 类 号：O557.63[理学—热学与物质分子运动论]