试论联用在线凝胶渗透色谱-气相色谱-三重四极杆质谱测定毒鼠强的效果  

Study on detection method for tetramine intoxication by on line GPC-GC-MS/MS

作　　者：劳哲[1] 江恩源[1] 

机构地区：[1]梧州市疾病预防控制中心,广西梧州543002

出　　处：《当代医药论丛》2017年第7期20-21,共2页

基　　金：梧州市公共突发事件处理专项经费项目资助

摘　　要：目的 :研究联用在线凝胶渗透色谱-气相色谱-三重四极杆质谱(GPC-GC-MS/MS)测定液、固体样品中毒鼠强含量的效果。方法 :将毒鼠强标准系列溶液中的6个特征离子(m/z 240、m/z 212、m/z 132、m/z121、m/z132、m/z149)作为母离子,使用3V^45V的电压对其进行碰撞处理,经产物离子优化后得到离子丰度较高的6个离子对(212→132;212→92;240→212;240→149;132→105;212→200)。将离子对丰度最高的离子对(212→132)作为定量离子对,将其余5个离子对作为定性离子对设为多反应监测(MRM)参数。标准液与样品同时进行提取、纯化、浓缩、定容,然后进行测定。结果 :标准曲线为:y=215232.7x+31 x+31,r=0.9996,回收率为:98.7%,RSD=4.5%,液体样品的检出限为0.00001mg/L,固体样品的检出限为0.00002mg/kg。结论 :联用在线凝胶渗透色谱-气相色谱-三重四极杆质谱测定毒鼠强标准系列溶液具有高效、准确性好、检出限低的特点。Objective To study the method for determination of tetramine intoxication by on line GPC-GC-MS/MS. Methods With the standard solution to tetramine 6 characteristic ions （m/z 240, m/z 212, m/z 132, m/z121, m/z132, m/z149） as parent ion, use 3V-45V voltage for collision, then got ion abundance high 6 ion pairs （212 → 132; 212 → 92; 240 → 212; 240 → 149; 132 → 105; 212 → 200）. After produced ion were optimized, set the highest ion pair （212 → 132） as the quantitative ion pair, set remained 5 ion pairs as qualitative ion pairs, set MSM parameter. Then to do extraction, purity, concentration, constant volume for standard liquid and sample in the same time, after that ,and do determination.Results Standard curve： y=215232.7x 31 x 31, r=0.999 6, recovery rate of 98.7%, RSD =4.5%, The detection limit of the liquid sample was 0.00001 mg/L, and the detection limit of the solid sample was 0.000 02 mg/kg. Conclusion The method for determination of tetramine intoxication by on line GPC-GC-MS/MS effective and exact, had low detection limit.

关 键 词：毒鼠强 准系列溶液 在线凝胶渗透色谱-气相色谱-三重四极杆质谱 多反应监测 

分 类 号：R657.7[医药卫生—外科学]