GC-MS法测定薯蓣皂苷元大鼠血药浓度

GC-MS determination of diosgenin in rats plasma

目的:建立用气相色谱-质谱检测法测定血浆中薯蓣皂苷元血药浓度的方法。方法:采用 HP-5MS 石英弹性毛细管色谱柱(30m×0.25mm×0.25μm),载气 he;流速1.0mL·min^(-1),气化室温度330℃,传输温度280℃,离子源温度为230℃,四极杆温度为150℃;进样方式:分流进样;柱升温程序:起始温度230℃,以24℃·min^(-1)的速率升温至250℃,以25℃·min^(-1)速率升温至300℃,保持23min,电离方式为 EI,能量70eV,倍增电压2580V,选择离子检测(SIM),选择 m/z 139和 m/z 124作为薯蓣皂苷元及内标物的靶离子,m/z 300和 m/z 302作为辅助定量离子。结果:薯蓣皂苷元浓度在0.013～1.67μg·mL^(-1)范围内线性关系良好。最低检测浓度为0.013μg·mL^(-1),血浆样品回收率为92.03%,日内及日间的精密度分别为2.9%及2.4%。结论:气相色谱—质谱法可检测大鼠血浆中薯蓣皂苷元的含量,方法简便、可靠、快速。

Objective： To develop a GC - MS method for the determination of diosgenin in plasma. Methods： HP - 5MS capillary column（30 m ×0. 25 mm ×0. 25 μm） ,gas was He at a flow rate 1.0 mL · min^ -1 ,injector temperature was 300 ℃, transfer temperature was 280 ℃, MS source temperature was 230 ℃, MS Quad temperature was 150 ℃, split injection, the colum temperature was 230 - 300 ℃ and rose gradually by the program as follow ： initial temperature was 230 ℃, rose to 250 ℃ at the rate 4 ℃· min^- 1, then rose to 300 ℃ at the rate 25 ℃ · min^-1, maintained 23 min. EI ionization, electric energy was 70 eV, multiplier voltage was 2580 V. Selected ion monitoring （SIM） was used as detector. Ions m/z 139 and m/z 124 were used as target ions of the diosgenin and the internal standard, respectively. Ions m/z 300 and m/z 302 were used as assistant quantitative ions. Results： The linear range of the diosgenin standard curve was 0. 013 - 1.67 μg · mL^-1 ,The detection limit was 0. 013 μg · mL^-1 ,The average recoveries of diosgenin was 92.03%. Precision of determination were 2.9% （ intra - day） and 2.4% （ inter -day） ,respectively. Conclusion：The method of GC -MS for determination of diosgenin in rats plasma is simple and reliable.