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目的:建立测定大鼠血浆中薯蓣皂苷元的液相色谱-质谱法(HPLC-MS)定量分析方法。方法:血浆样品加入内标丹参酮ⅡA(TanshinoneⅡA),酸化后用乙酸乙酯提取,进行HPLC-MS测定。色谱柱为ALLTIMA-C18(3.5μm,2.1mm×150mm),流动相为乙腈-0.1%三氟乙酸水溶液(95∶5),流速为0.2mL.min-1;采用HPLC-MS,选择离子监测(SIM)法检测薯蓣皂苷元([M+H]+,m/z415.4),丹参酮ⅡA(内标,[M+H]+,m/z295.2)。结果:血浆中杂质不干扰样品和内标的测定,线性范围为1～100μg·mL-1;方法回收率大于70%,日内、日间精密度RSD小于16%,稳定性符合生物样品测定要求。结论:经方法学确证和稳定性评价,该方法可用于薯蓣皂苷元的药动学研究。
Objective: To establish a method for the quantitative analysis of diosgenin in rat plasma by liquid chromatography-mass spectrometry (HPLC-MS). Methods: The plasma sample was added with Tanshinone Ⅱ A (internal standard), acidified and extracted with ethyl acetate for HPLC-MS. The column was ALLTIMA-C18 (3.5μm, 2.1mm × 150mm). The mobile phase was acetonitrile-0.1% trifluoroacetic acid (95: 5) and the flow rate was 0.2mL.min-1. The diosgenin ([M + H] +, m / z 415.4) and tanshinone IIA (internal standard, [M + H] +, m / z 295.2) were detected by SIM. Results: The impurity in plasma did not interfere with the determination of sample and internal standard. The linear range was 1 ~ 100μg · mL-1. The method recovery was more than 70%. The RSD of intra- and inter-day precision was less than 16% and the stability was in accordance with the determination of biological samples. Conclusion: The method can be used to study the pharmacokinetics of diosgenin by methodological confirmation and stability evaluation.