HPLC双波长法同时测定黄连上清片中栀子苷和盐酸小檗碱的含量

Determination of gardenia glycosides and berberine hydrochloride in Huanglian Shangging tablets by HPLC dual wavelength method

研究开发同时测定黄连上清片中栀子苷和盐酸小檗碱两种有效成分的定量方法。采用ZORBAX Eclipse XDB-C18(4.6×250mm,5μm)色谱柱,流动相:A泵为乙腈,B泵为0.2%磷酸,切换波长检测:0~10分钟检测栀子苷(λ=238nm)、10~50分钟检测盐酸小檗碱(λ=345nm),流速为1.0ml/min,梯度洗脱,柱温为30℃,进样10μL。可使各组分有效分离,栀子苷的回归方程:y=43651x-1027(r=0.9996)、加样回收率的平均值为98.95%(RSD=1.5%);盐酸小檗碱的回归方程:y=27519x-2836(r=0.9995)、加样回收率的平均值为99.07%(RSD=1.7%)。结果说明此法快速、专属性高,可用于对黄连上清片的质量控制。

An HPLC method was established for the simultaneous determination of gardenia glycosides and berberine bhydrochloride in Huanglian Shangqing Tablets.The chromatographic system was a ZORBAX Eclipse XDB-C18(4.6X 250mm,5μm)column with acetonitrile(A)-0.2%phosphoric acid(B)as the mobile phase,gradient elution and wavelengthswitching detection at 238nm for gardenia glycosides and 345nm for berberine hydrochloride,with a flow rate of 1.0ml/min and a column temperature of 30C and a sample volume of 7.5pl.The method can effectively separate the components,and the linearity of gardenia glucoside was good in the range of 0.0480~0.9600μg,and that of berberine hydrochloride was good in the range of 0.0730~1.460μg;the average recoveries of the two were 98.95%and 99.07%,and the RSDs were 1.5%and 1.7%,respectively.The method is rapid,accurate and can be used for the quality control of Huang Lian Shang Qing Tablets.