反相高效液相色谱法同时测定藏药五味黄连丸中6种有效成分的含量

Simultaneous Determination of 6 Kinds of Active Ingredients in Tibetan Medicine of Wuweihuanglian Pills by RP-HPLC

目的建立藏药五味黄连丸(黄连、红花、诃子、渣驯膏、麝香)中药根碱、表小檗碱、黄连碱、巴马汀、小檗碱和山柰素的RP-HPLC含量测定方法。方法采用RP-HPLC。Phenomenex ODS C18色谱柱(250×4.6mm,5μm);以乙腈-0.05mol·L-1磷酸二氢钾溶液(50∶50)(每100m L中加入十二烷基硫酸钠0.4g,再以磷酸调节p H值为4.0)为流动相;检测波长266nm;柱温35℃;流速1.0m L·min-1;结果线性范围分别为:药根碱1.5664~31.3284μg·mL^(-1)(r=0.9978),表小檗碱1.6987~33.9736μg·mL^(-1)(r=0.9973),黄连碱3.7294~74.5884μg·mL^(-1)(r=0.9993),巴马汀3.3976~67.95μg·mL^(-1)(r=0.9994),盐酸小檗碱22.7242~227.2424μg·mL^(-1)(r=0.9988),山柰素1.121~22.42μg·mL^(-1)(r=0.9990);平均回收率分别为:药根碱100.19%、(RSD=1.92%,n=6),表小檗碱98.74%(RSD=1.57%,n=6),黄连碱98.58%(RSD=1.22%,n=6),巴马汀100.47%(RSD=1.84%,n=6),小檗碱为101.28%(RSD=1.88%,n=6),山柰素为99.53%(RSD=1.97%,n=6)。结论本方法操作简便、快速,结果准确,可用于五味黄连丸的质量控制。

OBJECTIVE To estahlish a HPLC method for the simultaneous determination of jateorhizine,epiberberine,coptisine,palmatine,berberine and kaempferol in Tibetan medicine of Wuweihuanglian Pills(Coptidis Rhizoma,Carthamus Tinctorius,Myrobalan,Trogopterus Dung Cream,Musk) by QAMS.METHODS HPLC method was adopted.The Phenomenex ODS C18 colunm(250 mm × 4.6 mm,5μm) was used,The mobile phase of acetonitrile-0.05 mol·L^(-1) Potassium Phosphate Monobasic solution(50 ∶ 50)(0.4 g of sodium dodecyl sulfate was added per 100 mL,adjust pH to 4.0 with Phosphoric acid),The flow rate was 1.0 mL·min^(-1) with UV detection wavelength at 266 nm and the column temperature was maintained at 35℃.RESULTS The linear ranges of jateorhizine,epiberberine,coptisine,palmatine,berberine and kaempferol hydrochloride were in the range of 1.5664 ~ 31.3284μg ·mL^(-1)(r = 0.9973),in the range of 1.6987 ~ 33.9736μg·mL^(-1)(r = 0.9973),in the range of 3.7294 ~ 74.5884μg·mL^(-1)(r = 0.9993),in the range of 3.3976 ~ 67.95μg · mL^(-1)(r = 0.9994),in the range of 22.7242 ~227.2424μg·mL^(-1)(r = 0.9988),in the range of 1.121 ~ 22.42μg·mL^(-1)(r = 0.9990) with average recoveries of 100.19%(RSD was 1.92%,n = 6),98.74%(RSD was 1.57%,n = 6),98.58%(RSD was 1.22%,n = 6),100.47%(RSD was 1.84%,n = 6) and 101.28%(RSD was 1.88%,n = 6),99.53%(RSD was 1.97%,n = 6),respectively.CONCLUSION This method is simple fast and accurate,which is suitable for quality control of Wuweihuanglian Pills.