建立同时测定大鼠血浆中丹参素钠与原儿茶醛和咖啡酸、迷迭香酸和丹酚酸A含量的液质联用方法  

Simultaneous determination of sodium danshensu, protocatechualdehyde and caffeic acid,rosmarinic acid and salvianolic acid A in the plasma of rats by HPLC-MS/MS method

作　　者：郑英明[1,2] 仇琪[1,2] 曹飒丽[3] 付京[3] 尹兴斌[3] 刘文芳[1,2] 杨克旭[1,2] 曹景琳 倪健[3] 林阳[1,2] 

机构地区：[1]北京市心肺血管疾病研究所 [2]首都医科大学附属北京安贞医院药事部,北京100029 [3]北京中医药大学基础医学院,北京100029

出　　处：《中国临床药理学杂志》2015年第4期297-299,303,共4页The Chinese Journal of Clinical Pharmacology

基　　金：国家科技重大专项基金资助项目(2012ZX 09303016);国家自然科学基金资助项目(81403200);北京市科技成果转化和产业化项目统筹基金资助项目(2012年Z121100006112062);科研基地建设-心血管重大疾病防治协同创新中心基金资助项目(PXM2014_014226_000002);科研基地建设-重点实验室-省部共建心血管重塑相关疾病教育部重点实验室基金资助项目(PXM2014_014226_000012)

摘　　要：目的建立HPLC-MS/MS法测定丹参素钠、原儿茶醛、咖啡酸、迷迭香酸和丹酚酸A在大鼠血浆中浓度的方法。方法用乙腈蛋白沉淀法处理血浆样本,色谱柱为Synergi Hydro-RP 80 A（150 mm×2 mm,4μm）,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,0-2 min,10%-60%乙腈;2-3 min,60%-95%乙腈;3-6.5 min,95%乙腈;6.5-7 min,95%-10%乙腈;7-12 min,10%乙腈,流速为0.4 m L·min-1;电喷雾电离（ESI）离子源离子化,采用多重反应监测（MRM）方式进行负离子检测。结果丹参素钠、原儿茶醛、咖啡酸、迷迭香酸和丹酚酸A的线性范围分别为10-1000,5-500,2-200,5-500,10-1000ng·m L-1;定量下限分别为10,5,2,5,10 ng·m L-1。日内精密度（RSD）均小于8.31%,日间RSD均小于12.73%,提取回收率均大于50%。结论本检测方法专属性高,操作简便,稳定性好,可以同时准确地检测丹参素钠、原儿茶醛、咖啡酸、迷迭香酸和丹酚酸A的血药浓度。Objective To establish a HPLC- MS / MS method to determinate the concentration of sodium danshensu,protocatechualdehyde and caffeic acid, rosmarinic acid and salvianolic acid A in rat plasma.Methods The analytes were extracted by protein precipitation. Synergi Hydro- RP 80 A（ 2 mm × 150 mm,4 μm） column was used. An gradient mobile phase consisting of acetonitrile- 0. 1% formic acid in water,0 ~ 2 min,10% ~ 60% acetonitrile,2 ~ 3 min,60% ~ 95% acetonitrile,3 ~ 6. 5 min,95% acetonitrile,6. 5 ~ 7 min,95% ~ 10% acetonitrile,7 ~ 12 min,10% acetonitrile,flow velocity was 0. 4 m L·min^- 1.After electrospray ionization（ ESI）,multiple reaction ion monitoring（ MRM） mode was adopted to detect the negative ions. Results The linearity range were 10- 1000,5- 500,2- 200,5- 500,10- 1000ng·m L- 1respectively. The lower limit of quantitation of drugs were 10,5,2,5,10 ng · m L^- 1. Intra and inter precisions（ RSD） were less than8. 31% and 12. 73%. Extraction recoviries for sodium danshensu,protocatechualdehyde,caffeic acid,rosmarinic acid and salvianolic acid A were both greater than 50%. Conclusion This method was simple,high specificity,good stability with good repeatability. It could be used todeterminate the plasma concentration of sodium danshensu,protocatechualdehyde,caffeic acid,rosmarinic acid and salvianolic acid A correctly and coinstantaneously.

关 键 词：丹参素钠 原儿茶醛 咖啡酸 迷迭香酸 丹酚酸A 液质联用法 血药浓度 

分 类 号：R285.5[医药卫生—中药学] R969.1[医药卫生—中医学]