Ji Hye Young, Jeong Dong Won, Kim Young Hoon, Kim Hui-Hyun, Yoon Yoo-Seok, Lee Kang Choon, Lee Hye Suk
Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy and Phytofermentation Research Center, Wonkwang University, Iksan 570-749, Korea.
Rapid Commun Mass Spectrom. 2006;20(14):2127-32. doi: 10.1002/rcm.2573.
A rapid, sensitive and selective method for the determination of gabapentin in human plasma was developed using hydrophilic interaction liquid chromatography/tandem mass spectrometry (HILIC/MS/MS). The devised method involved protein precipitation with acetonitrile followed by separation on an Atlantis HILIC silica column using an acetonitrile/ammonium formate mobile phase (100 mM, pH 3.0) (85:15, v/v). Analytes were detected using an electrospray ionization mass spectrometer in the multiple-reaction monitoring mode. The standard curve was linear (r = 1.000) over the concentration range of 50.0-10000 ng/mL. The lower limit of quantification for gabapentin was 50.0 ng/mL (ca. 20 pg gabapentin) using a 10-microL plasma sample. The coefficients of variation and relative errors for intra- and inter-assay at four QC levels (i.e., 50.0, 125, 750, and 7500 ng/mL) were 4.7 to 9.4% and -4.1 to 1.6%, respectively. Absolute and relative matrix effects for gabapentin and metformin were practically absent. Gabapentin and metformin recoveries were 98.5% and 99.0%, respectively. This method was successfully applied to a bioequivalence study of gabapentin in humans.
采用亲水作用液相色谱/串联质谱法(HILIC/MS/MS)建立了一种快速、灵敏且选择性好的人血浆中加巴喷丁的测定方法。该方法先用乙腈进行蛋白沉淀,然后在Atlantis HILIC硅胶柱上,以乙腈/甲酸铵流动相(100 mM,pH 3.0)(85:15,v/v)进行分离。采用电喷雾电离质谱仪在多反应监测模式下检测分析物。加巴喷丁在50.0 - 10000 ng/mL浓度范围内标准曲线呈线性(r = 1.000)。使用10 μL血浆样品时,加巴喷丁的定量下限为50.0 ng/mL(约20 pg加巴喷丁)。四个质量控制水平(即50.0、125、750和7500 ng/mL)下批内和批间变异系数及相对误差分别为4.7%至9.4%和 -4.1%至1.6%。加巴喷丁和二甲双胍几乎不存在绝对和相对基质效应。加巴喷丁和二甲双胍的回收率分别为98.5%和99.0%。该方法成功应用于加巴喷丁在人体的生物等效性研究。