高效液相色谱指纹图谱结合多成分含量测定的孕康口服液质量评价研究  

Quality Evaluation of Yunkang Oral Liquid Based on HPLC Fingerprint and Multi-content Determination

作　　者：俞小娜 颜美秋 俞静静 苏洁[1] 陈素红[3] 黄君凤 吕圭源[1] YU Xiaona;YAN Meiqiu;YU Jingjing(School of Pharmaceutical Sciences,Zhejiang Chinese Medical University,Hangzhou(310053),China;Shaoxing Central Hospital)

机构地区：[1]浙江中医药大学药学院,杭州310053 [2]绍兴市中心医院 [3]浙江工业大学 [4]回音必集团浙江齐齐哈尔制药有限公司

出　　处：《浙江中医药大学学报》2023年第8期947-955,共9页Journal of Zhejiang Chinese Medical University

基　　金：浙江省重点实验室项目(2012E10002)。

摘　　要：[目的]建立孕康口服液高效液相色谱(high performance liquid chromatography,HPLC)指纹图谱及6种成分含量测定的方法,结合化学模式分析,为孕康口服液质量标准改进及综合质量评价提供参考。[方法]采用Welch Ultimate Plus C_(18)柱,以乙腈-0.1%磷酸溶液1 mL·min^(-1)梯度洗脱,柱温30℃。检测波长0~24 min,240 nm;24~39 min,316 nm;39~49 min,246 nm;49~60 min,212 nm,建立18批孕康口服液的指纹图谱,并进行相似度评价、聚类分析、主成分分析、正交偏最小二乘法判别分析,并在此基础上对口服液中的马钱苷等6种成分进行定量分析。[结果]指纹图谱标定共有峰19个,指认了其中6个色谱峰,18批样品的相似度≥0.982。聚类分析、主成分分析及正交偏最小二乘法判别分析均将18批样品按厂家来源归成2类,筛选出包括马钱苷和黄芩苷在内的10个质量差异标志峰。马钱苷、芍药苷、黄芩苷、补骨脂素、异补骨脂素、川续断皂苷Ⅵ在3.24~32.40、7.10~71.00、23.20~232.00、0.81~8.08、0.82~8.16、7.00~70.00μg·mL^(-1)范围内线性关系良好;精密度、稳定性、重复性相对标准偏差(relative standard deviation,RSD)<2.00%;平均加样回收率在97.04%~101.32%,RSD为1.21%~2.96%,含量分别为0.34~0.46、0.70~0.93、1.71~3.48、0.04~0.08、0.04~0.08、0.62~0.94 mg·mL^(-1)。[结论]本研究建立的HPLC指纹图谱及多成分含量测定结合化学计量法的孕康口服液质量评价体系,方法快速准确可靠,可用于孕康口服液的质量控制与评价。[Objective]To establish the high performance liquid chromatography(HPLC)fingerprint and content determination method of 6 components,combined with chemometrics,which can provide scientific evidence for the quality standard research of Yunkang Oral Liquid.[Methods]The separation was performed by HPLC equipped with a Welch Ultimate Plus C_(18) chromatographic column.Acetonitrile-0.1%phosphoric acid solution with gradient elution at the flow rate of 1 mL·min^(-1).The column temperature was 30℃.The detection wavelengths were 0~24 min,240 nm;24~39 min,316 nm;39~49 min,246 nm;49~60 min,212 nm.The HPLC fingerprint of 18 batches of Yunkang Oral Liquid was established and the data were analyzed by similarity evaluation,cluster analysis(CA),principal component analysis(PCA),orthogonal partial least squares-discriminate analysis(OPLS-DA).And based on this,quantitative analysis was conducted on 6 components including loganin in the oral liquid.[Results]There were 19 common peaks in the HPLC fingerprint and 6 of them were quantitatively analyzed of 18 batches of samples,and the similarity was over 0.982.The CA,PCA and OPLS-DA divided the 18 batches of samples into 2 categories.Meanwhile,10 quality difference marker peaks including loganin and baicalin were screened.The content determination results showed that the linear relationship was good within the ranges of 3.24~32.40,7.10~71.00,23.20~232.00,0.81~8.08,0.82~8.16,7.00~70.00μg·mL^(-1) for loganin,paeoniflorin,baicalin,psoralen,isopsoralen,asperosaponinⅥ.Relative standard deviation(RSD)of precision,stability and reproducibility tests were<2.00%,whose average recoveries were 97.04%~101.32%with the RSD of 1.21%~2.96%.The contents were 0.34~0.46,0.70~0.93,1.71~3.48,0.04~0.08,0.04~0.08,0.62~0.94 mg·mL^(-1),respectively.[Conclusion]The quality evaluation system of Yunkang Oral Liquid based on HPLC fingerprint and multi-content determination combined with chemometrics was established in this study,it’s fast,precise and reliable,which can use as a reference for the quali

关 键 词：孕康口服液 HPLC指纹图谱 相似度评价 聚类分析 主成分分析 正交偏最小二乘法判别分析 含量测定 质量评价 

分 类 号：R282[医药卫生—中药学]