脉络舒通颗粒HPLC指纹图谱及5个成分的含量测定  

HPLC Fingerprint and Content Determination of Five Components in Mailuo Shutong Granules

作　　者：范建伟 庄会芳 李蔚群 李艳芳 邱大伟 关永霞 张贵民 Fan Jianwei;Zhuang Huifang;Li Weiqun;Li Yanfang;Qiu Dawei;Guan Yongxia;Zhang Guimin(Lunan Hope Pharmaceutical Co.Ltd.,Shandong Linyi 276006,China;State Key Laboratory of Generic Manufacture Technology of Chinese Traditional Medicine,Lunan Pharmaceutical Group Co.Ltd.)

机构地区：[1]鲁南厚普制药有限公司,山东临沂276006 [2]鲁南制药集团股份有限公司中药制药共性技术国家重点实验室

出　　处：《中国药师》2021年第5期946-949,971,共5页China Pharmacist

基　　金：国家“重大新药创制”科技重大专项(编号:2018ZX09201010-005);临沂市自主创新重大专项(编号:2019ZDZX001);兰山区科技创新发展计划专项(编号:1811)。

摘　　要：目的:采用HPLC法建立脉络舒通颗粒指纹图谱,同时测定新绿原酸、绿原酸、隐绿原酸、芍药苷和盐酸小檗碱5个成分的含量,以全面评价和有效控制该制剂质量。方法:采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速:1.0 ml·min^(-1),检测波长:224 nm,柱温:30℃。结果:建立了脉络舒通颗粒的HPLC指纹图谱共有模式,12批样品的指纹图谱与共有模式相比较其相似度均大于0.94,确定了25个共有峰,并对其中5个共有峰进行了指认归属;新绿原酸、绿原酸、隐绿原酸、芍药苷和盐酸小檗碱分别在20.10~100.50μg·ml-1(r=0.9999)、54.70~273.50μg·ml-1(r=0.9999)、21.10~105.50μg·ml-1(r=0.9999)、65.80~329.00μg·ml-1(r=0.9998)、17.00~85.00μg·ml-1(r=0.9999)范围内线性关系良好,方法学考察结果亦显示各项指标均符合含量测定要求。结论:所建立的HPLC指纹图谱共有模式特征性强,多指标成分含量测定结合指纹图谱分析更能全面地表征脉络舒通颗粒的整体化学特征,藉此可有效地提升脉络舒通颗粒的质量控制水平。Objective:To establish a method for the fingerprint and quantitative analysis of five components(neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,paeoniflorin and berberine hydrochloride)in Mailuo Shutong granules by HPLC to evaluate and control the quality scientifically.Methods:The HPLC analysis was performed on a Kromasil C18 column(250 mm×4.6 mm,5μm)in a gradient elution program with acetonitrile-0.1%phosphoric acid solution as the mobile phase.The flow rate was1.0 ml·min^(-1),the detection wavelength was 224 nm and the column temperature was set at 30℃.Results:A common pattern of HPLC fingerprint of Mailuo Shutong granules was established.Compared with the common pattern,the similarities of 12 batches of samples were above 0.94 with 25 common peaks,and five of which were identified and assigned.The contents of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,paeoniflorin and berberine hydrochloride all showed good linear relationships within the range of 20.10-100.50μg·ml-1(r=0.9999),54.70-273.50μg·ml-1(r=0.9999),21.10-105.50μg·ml-1(r=0.9999),65.80-329.00μg·ml-1(r=0.9998)and 17.00-85.00μg·ml-1(r=0.9999),respectively.The results of methodology study also showed that all indexes met the requirements of content determination.Conclusion:The established common pattern of HPLC fingerprint of Mailuo Shutong granules has good characteristics.Combined with the fingerprint analysis,the content determination of multi index components can more comprehensively reflect the overall chemical characteristics of Mailuo Shutong granules,which will be conductive to promoting the quality control of the preparation.

关 键 词：脉络舒通颗粒 指纹图谱 新绿原酸 绿原酸 隐绿原酸 芍药苷 盐酸小檗碱 高效液相色谱法 

分 类 号：TQ460.72[医药卫生—药物分析学]