速效止泻胶囊定性定量检测方法研究

目的: 建立速效止泻胶囊的定性定量检测方法。 方法: 采用TLC法鉴别速效止泻胶囊中盐酸小檗碱和拳参;采用HPLC法测定处方中盐酸小檗碱含量及拳参中绿原酸含量。盐酸小檗碱色谱条件:依利特 Hypersil ODS₂(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-0.05 mol·L^-1磷酸二氢钾溶液-三乙胺(40: 60: 0.1)为流动相,流速1 mL·min^-1,紫外检测波长346 nm,柱温为30 ℃;绿原酸色谱条件:依利特Hypersil ODS₂(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-0.01 mol·L^-1磷酸二氢钾溶液-三乙胺-磷酸(7: 93: 0.4: 0.3)为流动相,流速1 mL·min^-1,紫外检测波长327 nm,柱温为30 ℃。 结果: 盐酸小檗碱和拳参薄层色谱定性鉴别特征明显;盐酸小檗碱与绿原酸含量测定,分别在2.0~6.0 μg(r=0.9992)和0.1~1.8 μg(r=0.9999)线性关系良好;平均回收率(n=6)分别为99.2%和102.3%,RSD分别为0.77%和1.3%。 结论: 本法可准确地定性、定量,有效地控制速效止泻胶囊的质量。

Objective: To establish the qualitative and quantitative detection method for Suxiao Zhixie capsules. Methods: Berberine hydrochloride and Bistortae Rhizoma in this preparation were identified by TLC.The contents of berberine hydrochloride and chlorogenic acid from Bistortae Rhizoma were determined by HPLC.The separation of berberine hydrochloride was performed on Hypersil ODS₂(4.6 mm×250 mm,5 μm)column,the mobile phase consisted of acetonitrile-0.05 mol·L^-1 monopotassium phosphate-triethylamine(40: 60: 0.1)with the flow rate of 1.0 mL·min^-1,and UV detection wavelength was 346 nm and column temperature was 30 ℃;The separation of chlorogenic acid was performed on Hypersil ODS₂(4.6 mm×250 mm,5 μm),the mobile phase consisted of acetonitrile-0.01 mol·L^-1 monopotassium phosphate-triethylamine-phosphoric acid(7: 93: 0.4: 0.3)with the flow rate of 1.0 mL·min^-1,and UV detection wavelength was 327 nm and column temperature was 30 ℃. Results: The TLC showed obvious features for the identification of berberine hydrocholoride and Bistoreae Rhizoma;Good linearities were obtained over the ranges of 2.0-6.0 μg(r=0.9992)for berberine hydrochloride,and 0.1-1.8 μg(r=0.9999)for chlorogenic acid;The average recoveries(n=6)of berberine hydrochloride and chlorogenic acid were 99.2%(RSD=0.77%)and 102.3%(RSD=1.3%). Conclusion: The methods of qualitative and quantitative analysis are accurate,and suitable for effectively quality control of Suxiao Zhixie capsules.

1 Drug Specifications Promulgated by the Ministry of Public Health,P R China(中华人民共和国卫生部标准中药成方制剂).Vol 13(第十三册).Standard Number(标准号):
2 LU Ri-gang(卢日刚),TANG Min-ling(唐敏玲),WEI Xiang-hong(韦向红),et al.RP-HPLC determination of berberine hydrochloride in Fukang cleaning solution(RP-HPLC法测定妇康洗液中盐酸小檗碱的含量).Chin J Pharm Anal(药物分析杂志),2002,22(3):195
3 HU Chun-1i(胡春丽),WANG Dong-mei(王冬梅),ZHANG Peng(张鹏),et al.RP-HPLC simultaneous determination of baicalin,palmatine hydrochloride and berberine hydrochloride in Dangguilonghui tablets(RP-HPLC法同时测定当归龙荟片中黄芩苷、盐酸巴马汀和盐酸小聚碱的含量).Chin J Pharm Anal(药物分析杂志),2008,28(12):2011
4 LIANG Bo(梁波),ZHANG Xiao-li(张小丽).Research advances on chemical constituents and pharmacological activities of Polygonum bistorta L.(中药拳参化学成分及药理活性研究进展).J Gansu Norm Coll(甘肃高师学报),2008,13(5):53
5 ZHANG Xing-hai(张星海),WANG Yue-fei(王岳飞).A comparative study on bioactivities of tea polyphenols and chlorogenic acid(茶多酚与绿原酸生物活性的比较研究).J Tea Sci(茶叶科学),2007(01):39
6 LIU Dong-ling(刘冬凌),HU Bo(胡波),XIONG Wen-bi(熊文碧).Determination of gallic acid in Suxiao Zhixie capsules by RP-HPLC(HPLC测定速效止泻胶囊中没食子酸的含量).West China J Pharm Sci(华西药学杂志),2007,22(2):214
7 XIONG Can-qiong(熊灿琼),WANG Yi-fei(王义飞),WU Juan(吴娟).Determination of berberine hydrochloride and gallic acid in Suxiao Zhixie capsules by HPLC(HPLC法测定速效止泻胶囊中盐酸小檗碱和没食子酸的含量).Chin Pharm Aff(中国药事),2008,22(10):899
8 LAI Xian-rong(赖先荣),LIU Hui-lian(刘惠莲).Research on determination of berberine hydrochloride in Suxiaozhixie capsule(速效止泻胶囊含量测定方法的初步研究).Mod Biomed Prog(现代生物医药进展),2006,6(10):57
9 ChP(中国药典).2005 Vol Ⅰ(一部):271