高效液相色谱-串联质谱法同时测定乳制品中莫奈太尔和莫奈太尔砜  

Simultaneous Determination of Monepantel and Monepantel Sulfone in Dairy Products by HPLC-MS/MS

作　　者：吴映璇[1,2] 姚仰勋 邵琳智[1,2] 欧阳少伦 WU Yingxuan;YAO Yangxun;SHAO Linzhi;OUYANG Shaolun(Guangdong Inspection and Quarantine Technology Center,Guangzhou 510623,China;Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province,Guangzhou 510623,China)

机构地区：[1]广东检验检疫技术中心,广州510623 [2]广东省动植物与食品进出口技术措施研究重点实验室,广州510623

出　　处：《理化检验（化学分册）》2018年第8期883-887,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广东省科技计划项目(2015A030401074;2014A040401064)

摘　　要：采用高效液相色谱-串联质谱法同时测定乳制品(奶粉或液态奶)中莫奈太尔和莫奈太尔砜的含量。奶粉样品(约0.5g)加2mL水涡旋振荡至溶解完全,上述奶粉样品溶液或约2mL的液态奶样品,经5mL饱和氯化钠溶液、18mL乙腈超声提取,提取液浓缩后经正己烷净化。以Inertsil C_8-3色谱柱为分离柱,以不同体积比的0.5mmol·L^(-1)乙酸铵溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾负离子源和多反应监测模式。莫奈太尔和莫奈太尔砜的质量浓度均在5.0μg·L^(-1)以内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.008~0.018μg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为79.5%~104%,测定值的相对标准偏差(n=6)为2.8%~5.9%。HPLC-MS/MS was applied to the simultaneous determination of monepantel and monepantel sulfone in dairy products （milk powder or liquid milk）. The milk powder sample （about 0. 5 g） was vortexed to dissolve completely in 2 mL of water. The above milk powder sample solution or about 2 mL of liquid milk sample was extracted ultrasonically with saturated sodium chloride solution （5 mL） and 18 mL of aeetonitrile. After concentration, the extract was purified with n-hexane. Inertsil C8-3 chromatographic column was used as stationary phase, and the mixture of 0. 5 mmol·L^-1 ammonium acetate solution and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of monepantel and monepantel sulfone were kept in the same range within 5.0μg·L^-1 , with detection limits （3S/N） in the range of 0. 008-0. 018 μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 79. 5%-104%, with RSDs （n：6） in the range of 2. 8%-5.9%.

关 键 词：高效液相色谱-串联质谱法 莫奈太尔 莫奈太尔砜 乳制品 

分 类 号：O657.63[理学—分析化学]