复方白头翁灌肠液质量标准研究

Quality Standard of Compound Baitouweng Enema Liquid

目的 建立复方白头翁灌肠液的质量标准。方法 采用薄层色谱法对方中白头翁、黄连、黄柏、木香等中药材进行定性鉴别;采用高效液相色谱法测定白头翁皂苷B_(4)和盐酸小檗碱的含量,色谱柱为Inertsustain C_(18)键合硅胶柱(250 mm×4.6 mm,5μm),流动相分别为乙腈-0.1%磷酸溶液(30∶70,V/V,白头翁皂苷B_(4))和乙腈-0.1%磷酸溶液(50∶50,V/V,盐酸小檗碱),检测波长分别为205 nm(白头翁皂苷B_(4))和254 nm(盐酸小檗碱),柱温分别为35℃(白头翁皂苷B_(4))和40℃(盐酸小檗碱),流速为1.0 mL/min,进样量为15μL。结果 薄层色谱图中,白头翁、黄连、黄柏、木香的特征斑点均显色清晰,且阴性对照无干扰。白头翁皂苷B_(4)、盐酸小檗碱的质量浓度分别在91.00~910.00μg/mL(R^(2)=0.999 4,n=6)和31.00~310.00μg/mL(R^(2)=0.999 5,n=6)范围内与峰面积线性关系良好;平均加样回收率分别为100.90%和98.93%,RSD分别为0.97%和1.09%(n=9);精密度、稳定性、重复性试验结果的RSD均小于2.0%。每1 mL复方白头翁灌肠液中分别含白头翁皂苷B_(4)0.288 mg、盐酸小檗碱0.076 21 mg。结论 所建立的方法操作简便、结果准确可靠,可用于复方白头翁灌肠液的质量控制。

Objective To establish a quality standard for Compound Baitouweng Enema Liquid.Methods Thin-layer chromatography (TLC) method was used for the qualitative identification of Pulsatillae Radix,Coptidis Rhizoma,Phellodendri Chinensis Cortex and Aucklandiae Radix in the prescription.High-performance liquid chromatography (HPLC) method was used for the content determination of pulchinenoside B_(4) and berberine hydrochloride,the chromatographic column was Inertsustain C_(18)bonded silica gel column (250 mm×4.6 mm,5μm),the mobile phases were acetonitrile-0.1%phosphoric acid solution (30∶70,V/V,pulchinenoside B_(4)) and acetonitrile-0.1%phosphoric acid solution (50∶50,V/V,berberine hydrochloride),the detection wavelengths were 205 nm (pulchinenoside B_(4)) and 254 nm (berberine hydrochloride),the column temperatures were 35℃(pulchinenoside B_(4)) and 40℃(berberine hydrochloride),the flow rate was 1.0 mL/min,and the injection volume was 15μL.ResultsThe TLC spots of Pulsatillae Radix,Coptidis Rhizoma,Phellodendri Chinensis Cortex and Aucklandiae Radix were clear without any interference from the negative references.The linear ranges of pulchinenoside B_(4)and berberine hydrochloride were91.00-910.00μg/mL(R^(2)=0.999 4,n=6) and 31.00-310.00μg/mL(R^(2)=0.999 5,n=6),respectively.The average recoveries of pulchinenoside B_(4) and berberine hydrochloride were 100.90%and 98.93%,with RSDs of 0.97%and 1.09%(n=9),respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%.Each 1 mL of Compound Baitouweng Enema Liquid contained 0.288 mg of pulchinenoside B_(4) and 0.076 21 mg of berberine hydrochloride.Conclusion The established method is simple,accurate and reliable,which can be used for the quality control of Compound Baitouweng Enema Liquid.