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目的:建立驱铅颗粒的质量标准。方法:采用薄层色谱(TLC)法对制剂中丹参、木香、黄连进行鉴别;采用高效液相色谱(HPLC)法测定制剂中盐酸小檗碱的含量,色谱柱:Hvpersil BDS C_(18)柱(200mm×4.6 mm,5μm)柱;流动相:乙腈-0.033mol·L~(-1)KH_2PO_4溶液(35:65);流速:1.0 ml,min~(-1);检测波长:345 nm;柱温:30℃。结果:TLC鉴别丹参酮Ⅱ_A、去氢木香烃内酯、盐酸小檗碱在薄层板上有清晰的斑点,分离效果良好。盐酸小檗碱含量在4.08～130.82μg·ml~(-1)浓度范围内线性关系良好(r=0.999 9),平均回收率为98.1%(RSD=1.46%,n=9)。3批样品中盐酸小檗碱含量分别为0.67,0.71,0.58 mg·g~(-1)。结论:所建立的薄层鉴别方法专属性强,定量方法简便,准确,可用于驱铅颗粒的质量控制。
Objective: To establish the quality standard of lead-removing particles. Methods: TLC, TLC and HPLC were used to identify the content of berberine hydrochloride in the preparation. The column was Hvpersil BDS C 18 Column (200 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.033 mol·L -1 KH 2 PO 4 solution (35:65), the flow rate was 1.0 ml min -1 and the detection wavelength was 345 nm Column temperature: 30 ℃. Results: TLC identification of tanshinone Ⅱ_A, dehydrocostus lactone, berberine hydrochloride in the TLC plate has a clear spot, the separation effect is good. The content of berberine in the range of 4.08 ~ 130.82μg · ml ~ (-1) was linear (r = 0.999 9), the average recovery was 98.1% (RSD = 1.46%, n = 9). The contents of berberine hydrochloride in three batches of samples were 0.67, 0.71 and 0.58 mg · g -1, respectively. Conclusion: The TLC identification method is specific and specific, and the method is simple and accurate. It can be used for the quality control of lead excretion particles.