LC-MS/MS法测定人血浆中加巴喷丁的浓度
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篇名: LC-MS/MS法测定人血浆中加巴喷丁的浓度
TITLE:
摘要: 目的:建立测定人血浆中加巴喷丁(GBP)浓度的方法。方法:血浆样品经甲醇沉淀蛋白后,以磺胺甲噁唑为内标,采用液相色谱-串联质谱法测定。色谱柱为Diamonsil C18,流动相为水(含0.05%甲酸)-甲醇,梯度洗脱,流速为1 mL/min,柱温为30 ℃,进样量为20 μL。采用电喷雾离子源,以多反应监测进行正离子扫描,用于定量分析的离子对分别为m/z 172.0→154.1(GBP)、m/z 279.0→124.0(内标)。结果:GBP血药浓度在13.4~10 720.4 ng/mL范围内线性关系良好(r=0.992 3,n=5),定量下限为13.4 ng/mL,最低检测限为4.0 mg/mL;日内、日间RSD均小于10%,相对误差为-4.93%~5.10%;提取回收率为86.2%~90.3%(RSD<5%,n=6),基质效应为87.6%~92.1%。采用该法测得10例癫痫患者体内GBP的血药浓度为2 075.19~4 078.87 ng/mL(n=20)。结论:本方法灵敏度高、专属性好、适用性强,可用于癫痫患者体内GBP的血药浓度监测及药动学研究。
ABSTRACT: OBJECTIVE: To establish a method for the concentration determination of gabapentin (GBP) in human plasma. METHODS: After precipitated by methanol, using sulfamethoxazole as internal standard, LC-MS/MS method was adopted. The determination was performed on Diamonsil C18 column with mobile phase consisted of water (containing 0.05% formic acid)-methanol using a gradient elution program at the flow rate of 1 mL/min. The column temperature was 30 ℃, and sample size was 20 μL. The ESI was equipped and quantitative analysis was operated in positive ion and MRM mode. The mass transition ion-pairs were followed as m/z 172.0→154.1(GBP) and m/z 279.0→124.0 (internal standard). RESULTS: The linear range of GBP was 13.4-10 720.4 ng/mL (r=0.992 3,n=5). The limit of quantitation was 13.4 ng/mL, and the minimum detection limit was 4.0 ng/mL. RSDs of inter-day and intra-day were all lower than 10%. Relative errors ranged -4.93%-5.10%. The recoveries ranged 86.2%-90.3%(RSD<5%,n=6), and matrix effects ranged 87.6%-92.1%. The plasma concentration of GBP in 10 epileptic patients ranged 2 075.19-4 078.87 ng/mL (n=20). CONCLUSIONS: The method is proved to be sensitive, specific, practical and suitable for plasma concentration monitoring and pharmacokinetic study of GBP in epileptic patients.
期刊: 2017年第28卷第32期
作者: 许萌,周春华,张雪宁,亢泽坤
AUTHORS: XU Meng,ZHOU Chunhua,ZHANG Xuening,KANG Zekun
关键字: 加巴喷丁;液相色谱-串联质谱;血药浓度;癫痫患者
KEYWORDS: Gabapentin; LC-MS/MS; Plasma concentration; Epileptic patients
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