von Unruh G E, Paar W D
J Chromatogr. 1985 Nov 29;345(1):67-76. doi: 10.1016/0378-4347(85)80136-5.
The new anti-epileptic drug oxcarbazepine is temperature-labile and decomposes under the conditions of gas chromatography, even when injected into a cooled, inert, fused-silica capillary column. In contrast, the trimethylsilyl derivative of oxcarbazepine is stable. The bis-trimethylsilyl derivatives of the enol of oxcarbazepine and of its active metabolite, 10-hydroxycarbazepine, and the tris-trimethylsilyl derivative of carbazepine-10,11-trans-diol can be synthesized easily at room temperature. Using the readily available carbamazepine as internal standard, a simple gas chromatographic assay was developed for the simultaneous routine measurement of these three compounds at therapeutic levels. This assay is ten times more sensitive to oxcarbazepine than the previously described high-performance liquid chromatographic assays. It involves a single-step solvent extraction, uses a fused-silica capillary column and a flame ionization detector. On processing 0.5 ml of plasma, limits of detection of 10 ng/ml were obtained for oxcarbazepine and 10-hydroxycarbazepine and a limit of detection of 25 ng/ml for carbazepine-10,11-trans-diol.
新型抗癫痫药物奥卡西平对温度不稳定，在气相色谱条件下会分解，即使注入冷却的惰性熔融石英毛细管柱中也是如此。相比之下，奥卡西平的三甲基硅烷基衍生物是稳定的。奥卡西平及其活性代谢物10-羟基卡马西平的烯醇式双三甲基硅烷基衍生物以及卡马西平-10,11-反式二醇的三叔甲基硅烷基衍生物在室温下可轻松合成。以易于获得的卡马西平作为内标，开发了一种简单的气相色谱分析法，用于同时常规测定治疗水平下的这三种化合物。该分析法对奥卡西平的灵敏度比先前描述的高效液相色谱分析法高十倍。它涉及一步溶剂萃取，使用熔融石英毛细管柱和火焰离子化检测器。处理0.5毫升血浆时，奥卡西平和10-羟基卡马西平的检测限为10纳克/毫升，卡马西平-10,11-反式二醇的检测限为25纳克/毫升。
