固相萃取/超高效液相色谱法测定龙胆泻肝丸中栀子苷、龙胆苦苷与黄芩苷  

Determination of Geniposide,Gentiopicroside and Baicalin in Longdanxiegan Pill by SPE/UPLC

作　　者：张勇[1] 薛昆鹏 何美 陈再洁 吴虹[1] 赵岳星 

机构地区：[1]安徽中医学院药学院,安徽合肥230031 [2]月旭材料科技(上海)有限公司,上海201203

出　　处：《分析测试学报》2013年第1期122-126,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(81073122);安徽中医学院自然科学基金项目(2012zr023)

摘　　要：建立了一种快速测定龙胆泻肝丸中栀子苷、龙胆苦苷和黄芩苷3种有效成分的超高效液相色谱方法。样品经50%甲醇提取,C18固相萃取(SPE)小柱净化后,采用Ultimate XB-C18色谱柱(4.6 mm×50 mm,1.8μm)进行分离,以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱。考察了不同规格色谱柱、流动相梯度比例、进样体积、柱温和流速对分离效果的影响,并对SPE柱流出液的平衡体积进一步考察,在最佳分析条件下进行液相色谱分析,该方法显示了良好的线性关系(r≥0.999 8),其定量下限(LOQ)为0.24～0.44 mg/L,加标回收率为95%～99%。该方法快速、准确,可满足实际检测需要。A rapid method for the determination of geniposide,gentiopicroside and baicalin in Longdanxiegan Pill was established.The sample was extracted with 50% methanol,and then purified with C18 solid phase extraction.The extract was separated on an Ultimate XB-C18（4.6 mm×50 mm,1.8 μm） column at 25 ℃,using acetonitrile-0.1% phosphate acid as mobile phase by gradient elution at flow rate of 0.8 mL·min-1.The effects of experimental conditions,such as different type of column,composition of mobile phase,injection volume,column temperature and flow rate,on separation efficiency of three compounds were investigated,and the equilibrium volume of SPE elution was also discussed.Under the optimal conditions,the method showed good linearity with correlation coefficients not less than 0.999 8.The quantitation limits（LOQs） were in the range of 0.24-0.44 mg/L,and the recoveries ranged from 95% to 99% with RSD no more than 2.8%.The method was rapid and reliable for the quantitation of three compounds in Longdanxiegan Pills.

关 键 词：龙胆泻肝丸 固相萃取 超高效液相色谱法 栀子苷 龙胆苦苷 黄芩苷 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]