中国临床药学杂志

目的建立LC-MS/MS法测定人血浆中卡马西平的浓度。方法以卡马西平-d2作为内标,血浆经甲醇直接蛋白沉淀后进样分析,色谱柱为CAPCELL PAK C18(100 mm×2.0 mm,5μm),流动相为甲醇-0.1 mmol·L-1乙酸铵水溶液(含0.02%乙酸)(70∶30),流速0.3 m L·min-1。电喷雾离子源,正离子多反应监测扫描分析。卡马西平和内标卡马西平-d2的离子对分别为m/z 237.1→194.1和m/z 239.1→196.1。结果卡马西平在质量浓度3.077 9¹ 231.2μg·L-1内线性良好(r=0.999 3,n=10);批内和批间精密度良好(RSD均<7.0%);提取回收率为98.94%~108.84%,RSD<15%;基质效应为92.76%~98.54%,RSD<5%。结论本方法灵敏度、重复性以及专属性均较好,样品处理简便易行,可用于卡马西平的血药浓度测定及药动学研究。

AIM To develop an LC-MS /MS method for determination of carbamazepine( CBZ) concentration in human plasma. METHODS With CBZ-d2 as internal standard and protein precipitated by methanol,the plasma samples were separated on CAPCELL PAK C18( 100 mm × 2. 0 mm,5 μm) column,and the mobile phase consisted of methanol-0. 1 mmol·L-1ammonium acetate solution( 0. 02% acetic acid)( 70∶ 30) at a flow rate of0. 3 m L·min-1. The detection of CBZ was performed in multiple reaction monitoring( MRM) mode using electrospray ionization( ESI+) source,monitoring the transition of the protonated molecular ion for CBZ at m/z 237. 1 and CBZ-d2 at m / z 239. 1 to the predominant ions of m / z 194. 1 and 196. 1,respectively. RESULTS The linear calibration curve of CBZ was obtained in the concentration range of 3. 077 9-1 231. 2 μg ·L-1( r = 0. 999 3,n =10). Both inter-batch RSD and intra-batch RSD were lower than 7. 0%. The average extraction recovery and matrix effect rates of CBZ were 98. 94%-108. 84%( RSD < 15%) and 92. 76%-98. 54%( RSD < 5%),respectively. CONCLUSION With the advantages of high sensitivity,good repeatability and specificity,the method is simple and suitable for determination of plasma concentration of CBZ and pharmacokinetic research.