超高效液相色谱-串联质谱法同时测定血清中12种抗癫痫药物

引用本文: 代静, 高乐虹, 彭方达, 于丽佳, 王朝东, 王玉平, 丁春光. 超高效液相色谱-串联质谱法同时测定血清中12种抗癫痫药物[J]. 色谱, 2020, 38(8): 900-905. doi: 10.3724/SP.J.1123.2019.12025 shu

Citation: DAI Jing, GAO Lehong, PENG Fangda, YU Lijia, WANG Chaodong, WANG Yuping, DING Chunguang. Simultaneous determination of twelve antiepileptic drugs in serum by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(8): 900-905. doi: 10.3724/SP.J.1123.2019.12025 shu

超高效液相色谱-串联质谱法同时测定血清中12种抗癫痫药物

代静 ^1, ,
高乐虹 ^2, ,
彭方达 ^1, ,
于丽佳 ^1, ,
王朝东 ^2, ,
王玉平 ^2, ,
丁春光 ^{1,
,}

1.
国家卫生健康委职业安全卫生研究中心, 北京 102308;
2.
首都医科大学宣武医院, 北京 100053

通讯作者: 丁春光, E-mail:13466322180@163.com

基金项目:
国家安全生产监督管理总局关键技术项目（2017005）；国家重点研发计划（2017YFC0907702）.

摘要: 建立了超高效液相色谱-串联质谱同时测定血清中加巴喷丁、拉莫三嗪、普瑞巴林、拉考沙胺、左乙拉西坦、托吡酯、奥卡西平、氯硝西泮、丙戊酸钠、卡马西平、苯巴比妥、苯妥英钠12种抗癫痫药物的方法。将非那西丁和氯唑沙宗分别作为正离子和负离子模式下的内标物，血清经乙腈沉淀蛋白质后，取上清液进样分析。采用ACQUITY UPLC BEH C₁₈柱分离，流动相为水和甲醇（均含10 mmol/L甲酸铵），流速为0.4 mL/min。采用电喷雾电离源，在多反应监测和正、负离子模式下分段进行扫描分析。结果表明，12种抗癫痫药物在各自范围内线性关系良好，相关系数均大于0.992，在3个添加水平下方法的加标回收率为90.80%~114.0%，批内精密度RSD≤13.2%，批间精密度RSD≤14.8%。该方法专属性强，灵敏度高，可用于12种抗癫痫药物临床血药浓度监测及药代动力学研究。

关键词:

English

Simultaneous determination of twelve antiepileptic drugs in serum by ultra high performance liquid chromatography-tandem mass spectrometry

1.
National Center for Occupational Safety and Health, Beijing 102308, China;
2.
Xuanwu Hospital Capital Medical University, Beijing 100053, China

Corresponding author: DING Chunguang, 13466322180@163.com

Received Date: 18 December 2019
Fund Project:
Key Technology Project of State Administration of Work Safety (No. 2017005)

Abstract: A sensitive, high-throughput method was established for the simultaneous determination of 12 antiepileptics in serum by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The antiepileptics were gabapentin, lamotrigine, pregabalin, lacosamide, levetiracetam, topiramate, oxcarbazepine, clonazepam, sodium valproate, carbamazepine, phenobarbital and phenytoin sodium. Phenacetin and chlorzoxazone were used as internal standards. The antiepileptics and internal standards were extracted from serum by protein precipitation using acetonitrile as the precipitant. Chromatographic separation was achieved on an ACQUITY UPLC BEH C₁₈ column with a gradient mobile phase comprising 10 mmol/L ammonium formate aqueous solution and methanol (containing 10 mmol/L ammonium formate) at a flow rate of 0.4 mL/min. Detection was performed in multiple reaction monitoring mode with ion mode switching. The results showed good linear trends in their respective concentration ranges and the correlation coefficients (r²) were greater than 0.992. The spiked recoveries of the 12 antiepileptics in serum were 90.80%-114.0% at the three spiked levels. The intra-assay (n=6) and inter-assay (n=3) precisions were less than 13.2% and 14.8%, respectively. The method has high specificity and sensitivity, and it can be used for clinical blood concentration monitoring and pharmacokinetic studies of the 12 antiepileptics.

Key words:

ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
/ blood drug concentration
/ antiepileptics
/ serum

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超高效液相色谱-串联质谱法同时测定血清中12种抗癫痫药物

通讯作者: 丁春光, E-mail:13466322180@163.com

English

Simultaneous determination of twelve antiepileptic drugs in serum by ultra high performance liquid chromatography-tandem mass spectrometry

Corresponding author: DING Chunguang, 13466322180@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联质谱法同时测定血清中12种抗癫痫药物

通讯作者: 丁春光, E-mail:13466322180@163.com

English

Simultaneous determination of twelve antiepileptic drugs in serum by ultra high performance liquid chromatography-tandem mass spectrometry

Corresponding author: DING Chunguang, 13466322180@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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