黄连解毒汤各成分的HPLC-UV/MS定性与定量测定方法研究  

Qualitative and quantitative determination of the main components of Huanglianjiedu decoction by HPLC-UV/MS

作　　者：孙健[1] 马吉胜[2] 金瑾[1] 王怀生[2] 温庆辉[1] 张宏桂[3] 周秋丽[1] 

机构地区：[1]吉林大学药学院,吉林长春130021 [2]吉林天药科技股份有限公司,吉林长春130012 [3]北京中医药大学中药学院,北京100102

出　　处：《药学学报》2006年第4期380-384,共5页Acta Pharmaceutica Sinica

摘　　要：目的建立可整体定性、多指标定量的黄连解毒汤的分析方法。方法使用HPLC-UV/MS方法,梯度洗脱黄连解毒汤样品及组方各药单煎样品,归属色谱峰来源,并对主要色谱峰进行定性、定量分析。采用Zorbax ExtendC18(150 mm×4.6 mm ID,5μm)色谱柱;流动相A为乙腈,B为水(含0.5%冰醋酸),流速1 mL.m in-1。紫外检测波长254 nm,正、负离子扫描获得质谱数据。结果归属了21个色谱峰的来源,发现两个可区分黄连、黄柏的特征峰,通过HPLC-UV/MS对其中11个主要色谱峰进行了指认,并以HPLC-UV对8种有对照品的成分进行含量评价。结论黄连解毒汤与组方各药单煎样品有较好相关性,建立的方法所测得液相色谱图特征性和专属性强,该方法结合含量测定为黄连解毒汤内在质量控制提供了更全面的信息。Aim To establish a comprehensive HPLC analytical method of Huanglianjiedu decoction. Methods This study was performed by HPLC-UV/MS to identify the chemical constituents of the whole and individual herbs of the ＂ Huanglianjiedu decoction＂. Zorbax Extend C18 （ 150 mm × 4.6 mm ID, 5 μm） column was used; the mobile phase was composed of acetonitrile （A） and water （B, with 0.5% acetic acid） with gradient elution; the flow rate was 1.0 mL ·min^-1 and the column temperature was setup at 25 ℃. The detection wavelength was 254 nm. Results The chromatogram of Huanglianjiedu decoction showed 21 main peaks. Peaks 1, 2, 5 and 18 were from Gardenia jasminoides Ellis, Peaks 8, 13, 14, 15, 16, 17, 19 and 21 from Scutellaria baicalensis Georgi. While 10 from Coptis chinensis Franch and 20 from PheUodendron amurense Rupr. , Peaks 3, 4, 6, 9, 11 and 12 came from them together. Peak 7 presented in the chromatograms of the herbs except Gardenia jasminoides Ellis. By comparison of the retention time, the on-line UV spectra and MS spectra, 11 peaks were identified as 5 （geniposide） , 9 （jatrorrhizine） , 10 （coptisine） , 11 （palmatine）, 12 （berberine） , 13 （baicalin） , 15 （oroxin A）, 17 （wogonoside） , 19 （ baicalein）, 20 （obaculactone） , 21 （wogonin） , then eight of them were quantified by HPLC-UV. Conclusion The method could represent the characteristics of Huanglianjiedu decoction, and it could be used to evaluate the quality and quantity of Huanglianjiedu decoction. It distinguished between Coptis chinensis Franch and Phellodendron amurense Rupr. by HPLC for the first time.

关 键 词：黄连解毒汤 HPLC-UV/MS 定性 定量 

分 类 号：R917[医药卫生—药物分析学]