基于多波长切换HPLC指纹图谱结合化学计量学和多指标含量测定的脉络舒通丸质量评价研究  

Quality Evaluation of Mailuoshutong Pills Based On Multi-Wavelength Switching HPLC Fingerprint Combined With Chemometrics and Multi-Indicator Content Determination

作　　者：孙玉 许丽丽 高文燕[4] 汪冰 李慧芬[1] 关永霞 孙仟 崔伟亮[1,2,5] 林永强 SUN Yu;XU Lili;GAO Wenyan;WANG Bing;LI Huifen;GUAN Yongxia;SUN Qian;CUI Weiliang;LIN Yongqiang(Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Shandong Provincial Institute for Food and Drug Control,jinan 250101,China;Shandong Academy of Innovation and Development,Jinan 271039,China;Otolaryngology Department,The People's Hospital of Xintai City,Taian 271200,China;National Key Laboratory of Integration and Innovation of Classic Prescriptions and Modern Traditional Chinese Medicine,Lunan Pharmaceutical Group,Linyi 276005,China)

机构地区：[1]山东中医药大学,济南250355 [2]山东省食品药品检验研究院,中药标准创新与质量评价工程实验室,济南250101 [3]山东省创新发展研究院,济南271039 [4]新泰市人民医院耳鼻喉科,山东泰安271200 [5]鲁南制药股份有限公司,经方与现代中药融合创新全国重点实验室,山东临沂276005

出　　处：《中国药学杂志》2024年第21期2065-2074,共10页Chinese Pharmaceutical Journal

基　　金：国家重点研发计划项目资助(2023YFC3504102);山东省重点研发计划项目资助(2021CXGC010511);泉城产业领军人才支持计划创新团队项目资助(MRJT2105);国家药品监管科学体系建设重点项目资助(RS2024Z006);山东中医药大学2022年教育教学研究课题资助(ZYY2022019)。

摘　　要：目的 建立指纹图谱和多指标定量与化学计量学相结合的脉络舒通丸质量评价方法。方法 采用Agilent ZORBAX SB-Aq C_(18)色谱柱(4.6 mm×250 mm, 5μm),柱温30℃,流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,检测波长(216、230、280、248、327、280、254 nm),流速为1.0 mL·min^(-1),建立脉络舒通丸指纹图谱,确定共有峰结合化学计量学分析,并对11种指标成分进行含量测定。结果 在指纹图谱研究中,标定了30个共有峰,通过对照品比对指认了12个成分,指纹图谱相似度范围均≥0.990;通过聚类分析、主成分分析、偏最小二乘判别分析等化学计量学综合分析,没食子酸、新绿原酸、隐绿原酸、绿原酸、芍药苷、盐酸黄柏碱、毛蕊异黄酮葡萄糖苷、异绿原酸A、异绿原酸C、哈巴俄苷、盐酸小檗碱是影响脉络舒通丸质量的主要因子,上述11种成分含量测定变化范围分别为0.62~0.84、1.45~2.50、1.30~2.78、3.35~5.28、2.44~4.02、0.54~0.88、0.16~0.23、0.61~0.76、1.39~1.76、0.41~0.54、2.28~3.34 mg·g^(-1)。经方法学验证,线性关系良好(r≥0.999 6),平均加样回收率为95.70%~104.90%,相对标准偏差(RSD)为0.62%~1.93%。结论 建立的多波长切换指纹图谱结合化学计量学分析与多指标含量测定方法稳定、可靠,为脉络舒通丸的质量控制、综合评价提供科学依据。OBJECTIVE To establish a quality evaluation method for Mailuoshutong Pills by combining fingerprints and multi indicator quantification combined with chemometrics.METHODS Agilent ZORBAX SB-Aq C_(18) chromatography column(4.6 mm×250 mm,5μm)was used,and the column temperature was maintained at 30℃.The mobile phase was acetonitrile-0.1%phosphoric acid aqueous solution.Gradient elution was carried out at a flow rate of 1.0 mL·min^(-1),and the detection wavelengths were 216,230,280,248,327,280 and 254 nm.The fingerprints of Mailuoshutong Pills(MLSTP)were established,the common peaks were determined combined with chemometric analysis,and the contents of 11 indicator components were determined.RESULTS A total of 30 common peaks were labeled in the fingerprints,and 12 components were identified through comparison with reference materials.The similarity of fingerprints of 16 batches of MLSTP were more than 0.990.Through cluster analysis,principal component analysis,and partial least squares discriminant analysis,it was found that gallic acid,neochlorogenic acid,cryptochlorogenic acid,chlorogenic acid,paeoniflorin,berberine hydrochloride,calycosin-7-glucoside,isochlorogenic acid A,isochlorogenic acid C,hapargoside,and berberine hydrochloride were the main factors affecting the quality of MLSTP,and the variation ranges of the content determination of the 11 components mentioned above were 0.62-0.84,1.45-2.50,1.30-2.78,3.35-5.28,2.44-4.02,0.54-0.88,0.16-0.23,0.61-0.76,1.39-1.76,0.41-0.54 and 2.28-3.34 mg·g^(-1),respectively.CONCLUSION The established multi-wavelength switching fingerprint spectrum combined with chemometric analysis and multi index content determination method is stable and reliable,which can provide scientific basis for the quality control and comprehensive evaluation of MLSTP.

关 键 词：脉络舒通丸 指纹图谱 化学计量学 含量测定 质量评价 

分 类 号：R917[医药卫生—药物分析学]