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-5430m×0.25mmi.d.交联石英毛细管柱。雷公藤甲素的质量浓度在1.0μg/L~50.0μg/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0.5μg/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。
A method for the determination of tiptolide in human plas ma bygas chromatography-electron capture detection is described. An SE-54 capillary column (30 m×0.25 mm i.d.) was used. N itroge n 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 anhy drid e. A good linearity was obtained from 1.0 μg/L to 50.0 μg/L of tiptolide in human plasma, r=0.999 0. The detection limit of it in plasma was 0.5 μg/L . The average recovery was 96.3%. The method is sensitive and precise.
参考文献
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