青蛤散质量控制研究

Study on the Quality Control for Qingge Powder

目的:建立青蛤散的质量控制方法。方法:采用TLC法鉴别青黛、关黄柏;限量测定升汞;HPLC法测定盐酸巴马汀、盐酸小檗碱的含量。色谱柱为Agilent ZORBAX SB-C18柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸溶液(磷酸二氢钠浓度为0.02 mol·L^(-1))为流动相,梯度洗脱,流速为0.8 ml·min^(-1),检测波长为345 nm,柱温为25℃,进样量为10μl。结果:青黛、关黄柏可在同一硅胶G薄层板进行薄层色谱鉴别;升汞可用比色法进行限量测定;盐酸巴马汀、盐酸小檗碱分别在0.020~0.205μg(r=0.999 6)和0.068~0.683μg(r=0.999 8)范围内呈良好的线性关系。加样回收率为98.17%～101.97%(RSD<2%,n=9)。结论:该方法简便,专属性强,稳定性好,可用于青蛤散的质量控制。

Objective： To establish the quality control for Qingge powder. Methods： TLC identification was performed for Indigo Naturalis and Phellodendri Amurensis cortex. Limit-determined test was used to detect mercury dichloride. An HPLC method was applied to determine the contents of palmatine hydrochloride and berberine hydrochloride with the following conditions： an Agilent ZORBAX SB-C18 chromatographic column（ 250 mm × 4. 6 mm,5 μm） was used,the mobile phase consisted of acetonitrile-0. 4% phosphoric acid（ the concentration of disodium hydrogen phosphate was 0. 02 mol · L^（-1）） with gradient elution at the flow rate of 0. 8 ml·min^（-1）,the detection wavelength was 345 nm,the column temperature was 25 ℃,and the injection volume was 10 μl. Results： Indigo Naturalis and Phellodendri Amurensis cortex could be identified by TLC at the same time. Mercury dichloride could be determined by colorimetry. The linear range of palmatine hydrochloride and berberine hydrochloride was 0. 020-0. 205 μg and 0. 068-0. 683 μg（ r =0. 999 6 and 0. 999 8）,respectively. The recoveries were ranged from 98. 17% to 101. 97%（ RSD 2%,n = 9）. Conclusion： The methods are simple and exclusive with good stability,which can be used as the quality control methods for Qingge powder.