液质联用法监测元胡止痛胶囊原料药的投料分析研究

The application of HPLC-MS/MS for comprehensively monitor the feeding analysis of Yuanhu analgesic capsules

目的 应用液质联用法（liquid chromatograph-massspectrometer, HPLC-MS/MS）监测元胡止痛胶囊中延胡索和白芷的投料情况，并同时检测其延胡索乙素、欧前胡素含量。方法 采用Inertsil ODS-3柱（4.6 mm×250 mm，5 μm），柱温40 ℃，流动相为0.1%甲酸-乙腈溶液，梯度洗脱，以HPLC法检测延胡索乙素、欧前胡素含量；采用电喷雾离子源负离子模式检测，选择多反应离子监测方式进行定性监测原料药的投料情况。结果 通过分析供试品与对照药材、对照品的一级质谱图相同的特征峰，可判断该中成药是按处方工艺投料；通过测定HPLC-MS/MS色谱峰面积，可对供试品进行定量。方法学验证结果表明，延胡索乙素和欧前胡素分别在5.08×10-5～30.45×10-5μg（r＝0.999 4）、5.02×10-5～30.09×10-5μg（r＝0.999 2）范围内呈良好线性关系；精密度试验RSD分别为0.99%、1.14%；回收率分别为97.02%～99.66%、97.62%～99.94%。结论 该法快速简便、灵敏度高、准确可靠，适用于全面监测元胡止痛胶囊中延胡索和白芷的投料情况及质量。

Objective The HPLC-MS/MS is used to comprehensively monitor the feeding conditions of raw materials in Yuanhu analgesic capsules, and the content of the index components can be detected at the same time. Methods The Inertsil ODS-3 （4.6 mm×250 mm, 5 mm） was used with the column temperature 40 ℃, Flow phase： 0.1% formic acid-acetonitrile; the gradient elution program, active ingredients were separated by HPLC, and the Electrospray Ionization Mass （ESI） source was applied and operated in the negative ion mode, and reactions ion monitoring mode （MRM） for quantitative analysis were selected. Results Through analysis and contrast of the medicinal materials, reference substance of primary mass spectrogram showed the same characteristic peak, and the proprietary Chinese medicine can be judged by prescription feeding process. The tetrahydroxene and imperatorin had a good linear relationship in 5.08×10-5-30.45×10-5μg （r=0.999 4）, 5.02×10-5-30.09×10-5 μg （r=0.999 2）. Precision test were 0.99% and 1.14%, the recovery rate were 97.02%-99.66%, 97.62%-99.94%. Conclusions The method is simple, accurate and reliable, high sensitive and fast. It is suitable to monitor the feeding condition and quality of yuanhu analgesic capsules.