利鼻片HPLC指纹图谱及多组分含量测定  

HPLC Fingerprint and Multi-component Content Determination of Libi Tablets

作　　者：梅璟妍 沈金花 MEI Jing-Yan;SHEN Jin-Hua(The Second Hospital of Yinzhou,Ningbo 315000,China;Ningbo TCM Hospital,Ningbo 315000,China)

机构地区：[1]浙江省宁波市鄞州区第二医院,浙江宁波315000 [2]浙江省宁波市中医院,浙江宁波315000

出　　处：《解放军药学学报》2024年第2期146-151,共6页Pharmaceutical Journal of Chinese People's Liberation Army

摘　　要：目的建立多组分含量测定结合化学计量学分析,评价利鼻片质量。方法采用高效液相色谱法,Waters SunFire C18色谱柱(4.6 mm×250 mm,5μm);乙腈(A)-0.55%磷酸水溶液(B)为流动相;梯度洗脱,流速:1.0 ml·min^(-1);切换检测波长:323、280、248 nm;柱温:35℃,进样量:10μl。采用中药色谱指纹图谱相似度评价系统结合聚类分析与正交偏最小二乘判别分析评价15批利鼻片质量。结果建立的利鼻片HPLC指纹图谱共确定了19个共有峰,并指认出其中7个色谱峰;利鼻片中菊苣酸、绿原酸、咖啡酸、黄芩苷、木兰脂素、欧前胡素、异欧前胡素的平均回收率分别为100.30%、99.87%、99.25%、99.45%、99.08%、98.75%和98.58%,RSD均<1.5%(n=6)。15批利鼻片中上述7个成分的含量测定结果分别为15.05~17.93、10.17~12.51、7.03~9.30、4.42~6.50、1.08~2.76、1.01~1.76、1.00~1.90 mg·g^(-1)。不同批次利鼻片存在差异,区分的特征峰为菊苣酸、绿原酸和木兰脂素。聚类分析结果表明3家企业的样品各自聚为一类,S1~S4(陕西康惠)聚为一类,S5~S10(通化民泰)聚为一类,S11~S15(长春银诺克)聚为一类。正交偏最小二乘法判别分析结果表明这4种化学成分〔10号峰菊苣酸(VIP值为2.216)、6号峰未知(VIP值为1.934)、4号峰绿原酸(VIP值为1.438)、13号峰木兰脂素(VIP值为1.013)〕显著影响利鼻片的分类,是引起该制剂质量差异的潜在标志性成分,可以考虑将这些差异标志性成分作为指标成分监控利鼻片的质量。结论建立的综合质量评价法简便、专属、准确,可客观评价利鼻片质量。Objective To evaluate the quality of Libi tablets by establishing a multi-component content determination method combined with chemometrics analysis.Methods HPLC was adopted on a Waters SunFire C18(4.6 mm×250 mm,5μm)column.The mobile phase was acetonitrile-0.55%phosphoric acid at a flow rate of 1.0 ml·min^(-1) with gradient elution.The detection wavelength was set at 323 nm,280 nm amd 248 nm respectively.The column temperature was 35℃and the injection volume was 10μl.The quality of 15 batches of Libi tablets was evaluated via the similarity evaluation system for chromatographic fingerprints of TCM combined with cluster analysis and principal component analysis.Results The results showed that 19 common peaks were identified,7 of which were peaks of chromatography.The average recoveries of chicoric acid,chlorogenic acid,caffeic acid,baical,magnolin,imperatorin,and isoimperatorin in Libi tablets were 100.30%,99.87%,99.25%,99.45%,99.08%,98.75%,98.58%,respectively,and the RSDs were all below 1.5%(n=6).The contents of the above 7 components in 15 batches of samples were 15.05―17.93,10.17―12.51,7.03―9.30,4.42―6.50,1.08―2.76,1.01―1.76,1.00―1.90 mg·g^(-1),respectively.Chemometric analysis showed that there was some difference between the samples of different batches.Significant characteristic peaks for discrimination between different samples were chicoric acid,chlorogenic acid and magnolin.The results of hierarchical cluster analysis showed that the samples from the three enterprises were grouped into one category respectively,namely S1-S4(Shaanxi Kanghui),S5-S10(Tonghua Mintai),and S11-S15(Changchun Yinnuoke).The results of orthogonal partial least square discriminant analysis(OPLS-DA)showed that these four chemical components〔peak 10(VIP value 2.216),peak 6(VIP value 1.934)unknown,peak 4(VIP value 1.438),peak 13(VIP value 1.013)〕made much difference to the categorization of Libi tablets,which were potential marker components that caused quality differences of the preparation and could be consid

关 键 词：利鼻片 菊苣酸 绿原酸 咖啡酸 黄芩苷 木兰脂素 欧前胡素 异欧前胡素 高效液相色谱法 化学计量学 

分 类 号：R927[医药卫生—药学]