LC-MS联用法测定人血浆中硫辛酸的浓度

Determination of Thioctic Acid in Human Plasma by LC-MS

目的:建立以液-质联用法测定人血浆中硫辛酸浓度的方法。方法:色谱柱为ZorbaxSBC18,流动相为甲醇∶乙腈∶0.1%冰醋酸(用氨水调节pH至4.0)=55∶10∶35,流速为0.3mL·min-1,内标为萘普生,柱温为40℃。采用选择性负离子(SIM)检测m/z205.0(硫辛酸)、m/z229.3(内标)。结果:硫辛酸检测浓度在0.01～10μg·mL-1范围内线性关系良好(r=0.9999);方法回收率在97.61%～106.31%之间,高、中、低3种浓度的日内和日间RSD均≤4%。结论:本方法灵敏、准确、重现性好,可用于硫辛酸的药动学和生物利用度研究。

OBJECTIVE：An LC- MS method was developed for the determination of thioctic acid in human plasma.METHODS： The chromatographic separation was carried out on Zorbax SB C18 column with the mobile phase consisting of methanol- acetonitrile-0.1% glacial acetic acid（adjusted pH to 4.0 with ammonia） （55 ： 10 ： 35） at a flow rate of 0.3mL · min^-1. Naproxen was used as internal standard .Column temperature was 40℃. SIM was used for determination of thioctic acid in human plasma. Ion mass spectral（m/z） of 205.0 was selected for thioctic acid and 229.3 for naproxen .RESULTS：The linear range of thioctic acid was 0.01 - 10μg · mL^-1（ r = 0.999 9）. The method recovery was within 97.61% - 106.31%. The intra - day and inter-day RED of thioctic acid（high, medium and low concentrations） were all less than 4% .CONCLUSION： The method is sensitive, accurate and reproducible, and suitable for the determination of thioctic acid in human plasma and its pharmacokinetic and bioavailability study.