复方白头翁灌肠液质量标准研究  

Quality Standard of Compound Baitouweng Enema Liquid

作　　者：陈平 罗晓梅[1] 曾于桦 杨强 张亚峰[1] 张鹏[1] CHEN Ping;LUO Xiaomei;ZENG Yuhua;YANG Qiang;ZHANG Yafeng;ZHANG Peng(Suining Central Hospital,Suining,Sichuan,China 629000)

机构地区：[1]四川省遂宁市中心医院,四川遂宁629000

出　　处：《中国药业》2023年第21期103-107,共5页China Pharmaceuticals

基　　金：四川省中医药管理局科学技术研究专项课题[2020CP0027,2021MS209]。

摘　　要：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.

关 键 词：复方白头翁灌肠液 白头翁皂苷B_(4) 盐酸小檗碱 薄层色谱法 高效液相色谱法 质量标准 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0