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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 |
| 阅读数： | 572 次 |
| 本月下载数： | 5 次 |
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