人血浆中左乙拉西坦和卡马西平同时测定方法的建立 点击下载
论文标题: 人血浆中左乙拉西坦和卡马西平同时测定方法的建立
英文标题:
中文摘要: 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。
英文摘要: 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
英文作者: 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-
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