上清丸黄柏中盐酸小檗碱含量测定及关黄柏掺伪或替代投料的检查

Determination of Berberine Hydrochloride and Inspection of Adulteration or Substitution of Phellodendron Chinense Cortex in Shangqing Pills by HPLC

目的:建立HPLC的方法测定上清丸盐酸小檗碱的含量,对市售上清丸中关黄柏掺伪或替代黄柏投料进行检查。方法:采用Waters xbridge C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-0.1%磷酸溶液(加入磷酸二氢钾使其达到0.02 mol/L)(20∶80)等度洗脱,流速为1 mL/min,柱温25℃,检测波长为345 nm。理论板数按盐酸小檗碱峰计算应不低于4000。结果:103批上清丸盐酸小檗碱含量存在差异,两种成分线性良好(r=1.0000),平均加样回收率为101.49%~105.53%(RSD值为1.5390~2.63%)。通过测定103批上清丸中盐酸小檗碱含量,上清丸(大蜜丸)中各企业样品含差异较小,上清丸(水丸)中L企业样品较M、N企业低。在上清丸中关黄柏掺伪或替代投料研究中,所有企业黄柏投料把关较严,盐酸巴马汀和盐酸小檗碱峰面积比值均小于0.05,未出现关黄柏掺伪或替代投料。结论:该分析方法简单可行,具有良好精密度、重复性和稳定性,为上清丸中黄柏质量评价提供参考。

Objective To establish a HPLC method for the determination of berberine hydrochloride in Shangqing pills,and to examine the adulteration or substitution of phellodendron chinense cortex in Shangqing pills.Methods Separation was performed on a Waters xbridge C_(18) column(250 mm×4.6 mm,5 μm) and the mobile phase was acetonitrile-0.1% phosphoric acid(potassium dihydrogen phosphate was added to reach 0.02 mol/L)(20∶80) with isocratic elution.The flow rate at 1 mL/min,the column temperature at 25 ℃,the detection wavelength at 345 nm,and the injection volume was 5 μL.Results The contents of berberine hydrochloride in 103 batches of Shangqing pills were different.There was a good linear relationships of two compoments in Shangqing Pills,with average recoveries of 101.49%-105.53%(RSD 1.53%-2.63%).The contents of berberine hydrochloride were little difference in Shangqing big honeyed pills produced by different enterprises,and the content of L enterprise samples were lower than that of M and N enterprise in Shangqing water honeyed pills.In the study on the adulteration or substitution of phellodendrus chinensis cortex in Shangqing pill,the ratio of peak area between palmatine hydrochloride and berberine hydrochloride were less than 0.05,and there was no adulteration or substitution of phellodendrus chinensis cortex.Conclusion The analytical method is simple and feasible,with good precision,repeatability and stability.The method can provide a reference for the quality evaluation of Shangqing Pills.