LC-MS法测定人血浆中丙戊酸钠的浓度  

Determination of Sodium Valproate Concentration in Human Plasma by LC-MS

作　　者：戴博 张华峰[1] 宋青[1] 梁贵键[1] 徐方楚[1] 

机构地区：[1]空军总医院药学部,北京100142

出　　处：《中国药房》2012年第22期2057-2058,共2页China Pharmacy

摘　　要：目的:建立测定人血浆中丙戊酸钠浓度的方法。方法:以霉酚酸为内标,血浆样品经乙腈直接沉淀蛋白后,采用液-质联用(LC-MS)法进样测定。色谱柱为Zorbax Eclipse XDB-C18,流动相为0.05%乙酸铵-乙腈(40:60),流速为0.2mL·min-1,柱温为30℃;通过电喷雾离子源(ESI)正负离子同时检测,丙戊酸钠、内标霉酚酸的检测离子分别为m/z166→143、m/z320→321。结果:丙戊酸钠血药浓度在2.5～200μg·mL-1范围内线性关系良好(r=0.9983),最低检测限为0.2μg·mL-1;高、中、低3种浓度的日内、日间RSD分别<3%、12%,方法回收率为105.5%～108.99%,绝对回收率均>70%。结论:本方法简便、快速、灵敏、准确,能够有效检测人血浆中丙戊酸钠的含量。OBJECTIVE：To establish a method for the determination of sodium valproate （VPA） in human plasma.METHODS：Mycophenolic acid was used as internal standard.After one step of protein precipitation with acetonitrile,LC-MS method was adopted.The determination was performed on a Eclipse XDB-C18 column with mobile phase consisted of 0.05% ammonium acetate-acetonitrile （40：60） at the flow rate of 0.2 mL·min-1.The column temperature was set at 30 ℃.The sample was determined by negative and positive ESI electrospray ionization source.The detection ions of sodium valproate and mycophenolic acid were m/z 166→143 and m/z 320→321.RESULTS：The linear range of sodium valproate was 2.5～200 μg·mL-1（r=0.998 3）.The lowest detection limit was 0.2 μg·mL-1.RSDs of intra-day and inter-day of three concentrations were less than 3% and 12%,respectively.The method recoveries were 105.5%～108.99%.The extraction recoveries were above 70%.CONCLUSION：The method is simple,rapid,sensitive and acourate,and it is suitable to determine the concentration of sodium valproate in human plasma.

关 键 词：液-质联用 丙戊酸钠 血药浓度 药动学 

分 类 号：R969.1[医药卫生—药理学] R971.6[医药卫生—药学]