HPLC测定人血浆中茴三硫浓度

HPLC Determination of Anethole Trithione in Human Plasma

目的:建立人血浆中茴三硫的 HPLC 测定方法。方法:用乙腈直接沉淀人血浆中的蛋白质,上清液在 Diamonsil ODS-C_(18)色谱柱(200mm×4.6mm,5μm)上,以甲醇-水(90:10)为流动相进行分离,流速1.0 mL·min^(-1),在346 nm波长处检测。结果:茴三硫与人血浆中的内源性物质完全分离且无其他干扰,保留时间约为3.7 min。线性范围为84～840 ng·mL^(-1),r=0.9999,高、中、低3种浓度血浆样品的日内 RSD 在2.3%～4.2%之间,日间 RSD 在2.6%～5.0%之间,回收率±SD(n=5)分别为95%±3.98%,95.74%±2.21%,98.78%±2.65%,血浆中茴三硫的最低定量浓度为84 ng·mL^(-1)。结论:所用方法简便、准确,重复性好,可用于茴三硫血浆样品的检测及药动学研究。

Objective： To establish an HPLC determination method for anethole trithione in human plasma. Method：Using acetonitrile to deposit protein directly, the anethole trithione and the impurity were separated on Diamonsil ODS - C18 column （200 mm × 4. 6 mm,5μm） with a mobile phase consisting of methanol - water （90： 10）, at a flow rate of 1.0 mL· min^- 1, the detection wavelength was 346 nm. Results： Anethole trithione was completely separated from the impurity, the retention time was 3.7 min. The calibration curve was linear within 84 -840 ng · mL^- 1 , r = 0. 9999. Within -day and between days, RSD were within 2. 3% -4.2% and 2.6% -5.0%, respectively. The recoveries of methodology ＋ SD （ n = 5 ） were 95%±3.98%, 95.74% ± 2.21%, 98.78% ± 2.65% for high, middle, and low content samples. The detection limit of anethole trithione in human plasma was 84 ng · mL^-1. Conclusion： This method is simple, accurate and reproducible.