气相色谱-质谱联用法定量测定人血清中的氨己烯酸和加巴喷丁。
Quantitative determination of vigabatrin and gabapentin in human serum by gas chromatography-mass spectrometry.
作者信息
Borrey Daniëlle C R, Godderis Kristof O, Engelrelst Veronique I L, Bernard Dirk R, Langlois Michel R
机构信息
Toxicology Unit, Department of Clinical Chemistry, AZ Sint-Jan AV, Ruddershove 10, B-8000 Brugge, Belgium.
出版信息
Clin Chim Acta. 2005 Apr;354(1-2):147-51. doi: 10.1016/j.cccn.2004.11.023. Epub 2005 Jan 13.
BACKGROUND
Published methods for routine clinical monitoring of vigabatrin and gabapentin are often very laborious. A simple GC-MS method was developed for the simultaneous quantitative determination of vigabatrin and gabapentin in human serum.
METHODS
After protein precipitation, the compounds are derivatized by methylation and analysed on a polydimethylsiloxane column using splitless injection. Cyclobarbital is used as the internal standard. To attain maximal sensitivity, detection is performed in selected ion monitoring mode.
RESULTS
The method was fully validated and linear calibration curves were obtained in the concentration ranges from 5 to 80 microg/mL for vigabatrin and from 5 to 30 microg/mL for gabapentin. The within-day and day-to-day relative standard deviations at three different concentration levels were <10% and <15%, respectively. The limit of quantitation was 2 mug/mL for both compounds.
CONCLUSIONS
The presented method provides high chromatographic resolution, good sensitivity and unequivocal identification potential and can be used for simultaneous analysis of both antiepileptics.
背景
已发表的用于氨己烯酸和加巴喷丁常规临床监测的方法通常非常繁琐。开发了一种简单的气相色谱 - 质谱法，用于同时定量测定人血清中的氨己烯酸和加巴喷丁。
方法
蛋白质沉淀后，化合物通过甲基化衍生化，并在聚二甲基硅氧烷柱上采用不分流进样进行分析。环巴比妥用作内标。为了获得最大灵敏度，在选择离子监测模式下进行检测。
结果
该方法得到充分验证，氨己烯酸在5至80μg/mL浓度范围内、加巴喷丁在5至30μg/mL浓度范围内获得线性校准曲线。在三个不同浓度水平下，日内和日间相对标准偏差分别<10%和<15%。两种化合物的定量限均为2μg/mL。
结论
所提出的方法具有高色谱分辨率、良好的灵敏度和明确的鉴定潜力，可用于同时分析这两种抗癫痫药物。
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