气相色谱-电子捕获法测定血浆中的雷公藤甲素

 血浆样品经碱化后用乙醚 氯仿 (体积比为 3∶1)混合液提取 ,浓缩的提取物与三氟醋酐进行衍生化反应 ,用气相色谱法分离、63Ni电子捕获检测器测定雷公藤甲素的含量。色谱柱为SE 5 430m× 0 2 5mmi d 交联石英毛细管柱。雷公藤甲素的质量浓度在 1 0 μg/L～ 5 0 0 μg/L范围内与峰面积线性关系良好 (r =0 9990 ) ,在血浆中的平均回收率为 96 3% ,最小检测限为 0 5 μg/L。方法重现性好 ,准确、灵敏 ,无杂质干扰 ,数据准确可靠 ,可用于临床生物样品中雷公藤甲素含量的测定。

Determination of Tiptolide in Human Plasma by Gas Chromatography-Electron Capture Detection

A method for the determination of tiptolide in human plasma by gas chromatography-electron capture detection is described. An SE-54 capillary column (30 m x 0.25 mm i.d.) was used. Nitrogen was used as the carrier gas. After NaOH solution being added, the plasma was extracted with ether-chloroform (3:1, V/V) and then reacted with trifluoroacetic anhydride. A good linearity was obtained from 1.0 microgram/L to 50.0 micrograms/L of tiptolide in human plasma, r = 0.9990. The detection limit of it in plasma was 0.5 microgram/L. The average recovery was 96.3%. The method is sensitive and precise.