LC-MS/MS检测血浆中黄连吴茱萸药对生物碱的研究

目的：快速准确测定黄连-吴茱萸药对中生物碱的血药浓度。方法：采用高效液相色谱-质谱联用法对黄连-吴茱萸药对中盐酸小檗碱、盐酸巴马汀、盐酸药根碱和吴茱萸碱的血药浓度进行测定,以甲醇-水为流动相梯度洗脱,Hypersil GOLD C18柱（50 mm×2.1 mm,3μm）为固定相,流速为0.2 ml/min,柱温为35℃。质谱采用高温电喷雾离子源,以选择反应监测模式进行定量分析,血浆样品用乙腈直接沉淀处理。结果：盐酸小檗碱在1.243～30.578 ng/ml,盐酸巴马汀在1.240～30.541 ng/ml,盐酸药根碱在1.248～30.647 ng/ml,吴茱萸碱在28.432～553.314 ng/ml范围内均呈良好线性关系。日内、日间RSD均小于15%（n=5）。结论：本方法操作简单、灵敏度高、分析时间短,适用于黄连-吴茱萸药对生物碱血药浓度监测及药代动力学研究。

LC-MS/MS Rapid Determination of the Alkaloid for Coptis-Evodia couplet medicines in Plasma

Objective:To determine the content of Alkaloid for Coptis-Evodia couplet medicines in plasma by LC-MS/MS.Methods:A high performance liquid chromatography electrospray mass spectrometry method for rapid determination of Berberine hydrochloride,Palmatine hydrochloride,Jatrorrhizine hydrochloride and Evodiamine for Coptis-Evodia couplet medicines in plasma has been established.The analysis was carriedon a Hypersil GOLD C18(50 mm×2.1 mm,3 μm) column.The column temperature was 35℃,with linear gradient elution using water and methanol,and the flow rate was 0.2 ml/min.The quantitation was done by selected reaction recording(SRM) mode of heater electrospray ionization(HESI),with phenytoin sa internal standard.Plasma was deposited by acetonitrile directly.Results:The linear range were 1.243~30.578 ng/ml for Berberine hydrochloride,1.240~30.541 ng/ml for Palmatine hydrochloride,1.248~30.647ng/ml for Jatrorrhizine hydrochloride and 28.432~553.314 ng/ml for Evodiamine;both intra-and inter-day RSD were less than 15%(n=5).Conclusion:The method is accurate,sensitive,simple,and suitable for study of therapeutic drug monitoring and pharmacokinetic.