LC-MS/MS法同时测定拉考沙胺和吡仑帕奈的血浆药物浓度 点击下载
| 论文标题： | LC-MS/MS法同时测定拉考沙胺和吡仑帕奈的血浆药物浓度 |
| 英文标题： | |
| 中文摘要： | 目的 建立同时测定人血浆中2种第三代抗癫痫药拉考沙胺和吡仑帕奈血浆药物浓度的方法并应用于临床。方法10例癫痫患者的血浆样品经乙腈沉淀蛋白并以乙腈-水（20∶80，V/V）稀释后，以氯氮平为内标，采用液相色谱-串联质谱法测定拉考沙胺、吡仑帕奈的质量浓度，再通过稀释倍数换算得血浆药物谷浓度。以WelchUltimateXB-C18为色谱柱，以10mmol/L甲酸铵溶液为流动相A、甲醇-乙腈-异丙醇（0.2%甲酸）混合溶液（7∶1.5∶1.5，V/V/V）为流动相B进行梯度洗脱，流速为0.4mL/min，柱温为40℃，进样量为5μL；采用电喷雾离子源以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/z251.2→144.1（拉考沙胺）、m/z350.2→219.2（吡仑帕奈）、m/z327.2→270.0（内标）。结果拉考沙胺、吡仑帕奈检测质量浓度的线性范围分别为0.00125～0.125μg/mL（r＞0.99）、0.0375～3.75ng/mL（r＞0.99），定量下限分别为0.00125μg/mL、0.0375ng/mL；批内、批间精密度，准确度，提取回收率，基质效应，稳定性均符合相关要求。1～5号患者体内拉考沙胺的谷浓度为5.3～12.2μg/mL，6～10号患者体内吡仑帕奈的谷浓度为208～510ng/mL。结论所建方法操作简便、快速，可用于拉考沙胺和吡仑帕奈的治疗药物监测。 |
| 英文摘要： | OBJECTIVE To establish a method for simultaneous determination of two third-generation anti-epileptic medicines such as lacosamide and perampanel in human plasma and apply this method in clinical practice. METHODS Using clozapine as internal standard， the concentrations of lacosamide and perampanel of plasma samples in 10 epileptic patients were determined by LC-MS/MS after protein precipitation with acetonitrile and dilution with acetonitrile-water （20∶80，V/V）， and the plasma minimum concentrations were obtained by dilution of multiple. The determination was performed on Welch Ultimate XB-C18 column， with mobile phase A consisted of 10 mmol/L ammonium formate and mobile phase B consisted of methanol-acetonitrile-isopropanol （0.2% formic acid） mixed solution （7∶1.5∶1.5， V/V/V） for gradient elution at the flow rate of 0.4 mL/min. The column temperature was set at 40 ℃ ， and the sample size was 5 μL. The electrospray ion source and multi-reaction monitoring mode were used for positive iron scanning. The ion pair used for quantitative analysis of lacosamide， perampanel and internal standard were m/z 251.2→ 144.1， m/z 350.2→219.2 and m/z 327.2→270.0， respectively. RESULTS The linear ranges of lacosamide and perampanel were 0.001 25-0.125 μg/mL（r＞0.99）， 0.037 5-3.75 ng/mL （r＞0.99）； the limits of quantification were 0.001 25 μg/mL and 0.037 5 ng/mL， respectively. The precision and accuracy within and between batches， extraction recovery rate， matrix effect， and stability all met relevant requirements. The minimum concentrations of lacosamide in No. 1-5 patients were 5.3-12.2 μg/mL， and the minimum concentrations of perampanel in No.6-10 patients were 208-510 ng/mL， respectively. CONCLUSIONS The established method is simple， rapid and suitable for the therapeutic drug monitoring of lacosamide and perampanel. |
| 期刊： | 2023年第34卷第16期 |
| 作者： | 余恒毅；徐艳娇；向东；刘璐；李喜平；刘东；贡雪芃 |
| 英文作者： | YU Hengyi，XU Yanjiao，XIANG Dong，LIU Lu，LI Xiping，LIU Dong，GONG Xuepeng |
| 关键字： | 拉考沙胺；吡仑帕奈；血浆药物浓度；治疗药物监测；液相色谱-串联质谱法 |
| KEYWORDS： | lacosamide； perampanel； plasma concentration； |
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