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人血浆中左乙拉西坦和卡马西平同时测定方法的建立
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| 篇名： | 人血浆中左乙拉西坦和卡马西平同时测定方法的建立 |
| TITLE： | Establishment of the method for simultaneous determination of levetiracetam and carbamazepine in human plasma |
| 摘要： | 目的 建立同时测定人血浆中左乙拉西坦和卡马西平浓度的方法。方法血浆样品经甲醇沉淀蛋白后，以卡马西平-D10为内标，采用高效液相色谱-串联质谱法测定其中左乙拉西坦和卡马西平的浓度。以XBridgeBEHC18为色谱柱，以甲醇-0.1％甲酸溶液为流动相进行梯度洗脱，流速为0.35mL/min，柱温为40℃，进样量为2μL；离子源为电喷雾离子源，采用多反应监测模式进行正离子扫描，用于定量分析的离子对分别为m/z171.3→126.3（左乙拉西坦）、m/z237.1→194.1（卡马西平）、m/z247.1→204.1（内标）。结果左乙拉西坦和卡马西平检测质量浓度的线性范围分别为0.5～50、0.2～20μg/mL（r分别为0.9973、0.9985），定量下限分别为0.5、0.2μg/mL；日内、日间RSD均不高于10.00％，日内、日间RE均在±4.00％之内，平均提取回收率为95.60％～105.00％，平均内标校正基质因子为98.40％～110.00％，稳定性试验的RSD均不高于5.60％。采用该法测得22例患者血浆中左乙拉西坦、卡马西平的浓度分别为3.36～40.90、3.64～9.93µg/mL。结论所建同时测定人血浆中左乙拉西坦、卡马西平浓度的高效液相色谱-串联质谱法快速、灵敏、准确、稳定，可用于癫痫患者血药浓度监测和药动学研究。 |
| ABSTRACT： | OBJECT IVE To e stablish the method for simultaneous determination of levetiracetam and carbamazepine concentrations in human plasma. METHODS After plasma samples were precipitated with methanol ，using carbamazepine-D 10 as the internal standard ，the concentrations of levetiracetam and carbamazepine were determined by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. The determination was performed on XBridge BEH C 18 column with methanol-0.1％ formic acid as mobile phase （gradient elution ）at the flow rate of 0.35 mL/min. The column temperature was set at 40℃，and sample size was 2 μL. With electrospray ion source，a multiple reaction monitoring mode was used for positive ion scanning；the detected ion pairs for quantitative analysis were m/z 171.3→126.3（levetiracetam），m/z 237.1→194.1（carbamazepine）， 247.1→204.1（internal standard ）. RESULTS The linear range of the concentrations of levetiracetam and carbamazepine were 0.5-50 and 0.2-20 μg/mL（r＝0.997 3 and 0.998 5），respectively；the lower quantitative limits were 0.5 and 0.2 μg/mL，respectively. RSDs of intra-day and inter-day were all no more than 10.00％. RE of intra-day and inter-day were within ±4.00％；the average extraction recoveries rate were 95.60％-105.00％；the average internal standard correction matrix factors were 98.40％-110.00％； RSDs of stability tests were all not higher than 5.60％. The concentrations of levetiracetam and carbamazepine in the plasma of 22 patients measured by this method were 3.36-40.90 and 3.64-9.93 μg/mL，respectively. CONCLUSIONS The established method for determining the concentration of levetiracetam and carbamazepine in human plasma is f ast，sensitive，accurate and stable ，and can be used for the monitoring of plasma concentration and pharmacokinetic study in epilepsy patients. |
| 期刊： | 2022年第33卷第08期 |
| 作者： | 史敏，任炳楠，吴惠珍，刘平，吴茵 |
| AUTHORS： | SHI Min，REN Bingnan ，WU Huizhen ，LIU Ping，WU Yin |
| 关键字： | 左乙拉西坦；卡马西平；血药浓度；高效液相色谱-串联质谱法 |
| KEYWORDS： | levetiracetam；carbamazepine；plasma concen- |
| 阅读数： | 246 次 |
| 本月下载数： | 3 次 |
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