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目的建立同时测定人血浆中苯巴比妥、苯妥英钠、托吡酯及左乙拉西坦浓度的方法。方法以磺胺甲噁唑(SMZ)和吡格列酮为内标,血浆经甲醇直接沉淀后进样分析。色谱柱为ACQUITY UPLC HSS PFP柱,流动相为含0.1%甲酸的5 mmol·L-1乙酸铵水溶液-甲醇溶液,流速为0.2 mL·min-1,电喷雾离子源,用多反应监测,结合正负离子分段扫描分析。结果苯巴比妥、苯妥英钠、托吡酯及左乙拉西坦血药浓度分别在1.15~230.00(r=0.997 3),0.10~20.20(r=0.998 5),0.02~2.12(r=0.996 5),0.10~20.40μg·mL-1(r=0.996 3)内线性关系良好。日内、日间精密度(RSD)均<15%;提取回收率均>75%。结论该方法灵敏、快速、专属性强,可用于临床血药浓度测定及药代动力学研究。
Objective To establish a method for simultaneous determination of phenobarbital, phenytoin, topiramate and levetiracetam in human plasma. Methods Sulfamethoxazole (SMZ) and pioglitazone were used as internal standards. The plasma was directly precipitated by methanol and then injected for analysis. The column was an ACQUITY UPLC HSS PFP column with a mobile phase of 5 mmol·L -1 ammonium acetate in methanol containing 0.1% formic acid at a flow rate of 0.2 mL · min -1. The electrospray ionization was monitored by multiple reaction monitoring Positive and Negative Ion Segment Scanning Analysis. Results The plasma concentrations of phenobarbital, phenytoin sodium, topiramate and levetiracetam were in the range of 1.15-230.00 (r = 0.9973), 0.10-20.20 (r = 0.998 5), 0.02-2.12 (r = 0.996 5) , 0.10 ~ 20.40μg · mL-1 (r = 0.996 3) within a good linear relationship. Intra-day and inter-day precision (RSD) were <15%; extraction recovery were> 75%. Conclusion The method is sensitive, rapid and specific, and can be used for the determination of clinical plasma concentration and pharmacokinetics.