Forrest G, Sills G J, Leach J P, Brodie M J
University Department of Medicine and Therapeutics, Western Infirmary, Glasgow, UK.
J Chromatogr B Biomed Appl. 1996 Jun 7;681(2):421-5. doi: 10.1016/0378-4347(96)00074-6.
A rapid and simple method for determination of the novel antiepileptic compound gabapentin [1-(aminomethyl)cyclohexaneacetic acid] in plasma is described. Blank human plasma was spiked with gabapentin (1.0-10.0 micrograms/ml) and internal standard [1-(aminomethyl)-cycloheptaneacetic acid; 5.0 micrograms/ml]. Individual samples were treated with 2 M perchloric acid, centrifuged and then derivatised with o-phthalaldehyde-3-mercaptopropionic acid. Separation was achieved on a Beckman Ultrasphere 5 microns reversed-phase column with mobile phase consisting of 0.33 M acetate buffer (pH 3.7; containing 100 mg/l EDTA)-methanol-acetonitrile (40:30:30, v/v). Eluents were monitored by fluorescence spectroscopy with excitation and emission wavelengths of 330 and 440 nm, respectively. The calibration curve for gabapentin in plasma was linear (r = 0.9997) over the concentration range 1.0-10.0 micrograms/ml. Recovery was seen to be > or = 90%. The inter- and intra-assay variations for three different gabapentin concentrations were < or = 10% throughout. The lower limit of quantitation was found to be 0.5 microgram/ml. Chromatography was unaffected by a range of commonly employed antiepileptic drugs or selected amino acids.
本文描述了一种快速简便的测定血浆中新型抗癫痫化合物加巴喷丁[1-(氨甲基)环己烷乙酸]的方法。将空白人血浆加入加巴喷丁(1.0 - 10.0微克/毫升)和内标[1-(氨甲基)环庚烷乙酸;5.0微克/毫升]。各个样品用2M高氯酸处理,离心,然后用邻苯二甲醛-3-巯基丙酸进行衍生化。在贝克曼Ultrasphere 5微米反相柱上进行分离,流动相由0.33M乙酸盐缓冲液(pH 3.7;含有100毫克/升乙二胺四乙酸)-甲醇-乙腈(40:30:30,v/v)组成。洗脱液通过荧光光谱法监测,激发波长和发射波长分别为330纳米和440纳米。血浆中加巴喷丁的校准曲线在1.0 - 10.0微克/毫升浓度范围内呈线性(r = 0.9997)。回收率≥90%。三种不同加巴喷丁浓度的批间和批内变异始终≤10%。定量下限为0.5微克/毫升。色谱分析不受一系列常用抗癫痫药物或选定氨基酸的影响。