高效液相色谱指纹图谱结合化学计量学方法分析不同产地侗药四块瓦药材质量  

Analysis of Quality of Dong Medicine Sikuaiwa from Different Origins by High Performance Liquid Chromatography Fingerprint Combined with Chemometrics

作　　者：徐玉平[1] 宋伟[2] 张德庆 滕乐 唐军相 赵昌涵 韩忠耀[2] XU Yuping;SONG Wei;ZHANG Deqing;TENG Le;TANG Junxiang;ZHAO Changhan;HAN Zhongyao(Kaili University,Kaili 556011,China;Qiannan Medical College for Nationalities,Duyun 558000,China)

机构地区：[1]凯里学院,凯里556011 [2]黔南民族医学高等专科学校,都匀558000

出　　处：《理化检验（化学分册）》2024年第9期872-877,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：贵州省自然科学技术基金(黔科合基础[2020]1Y390号);黔东南州科技计划项目(黔东南科合J字[2022]30号);贵州省2023年省级“金课”项目(SJJK202346);黔南民族医学高等专科学校科研基金项目(qnyz2024002);凯里学院2022年扶持市(州)高校质量提升工程项目(JXTD202202)。

摘　　要：取1 g四块瓦粉末置于圆底烧瓶中,加入75%(体积分数,下同)甲醇溶液50 mL,回流提取1 h,过滤,滤液用75%甲醇溶液定容至50 mL,经0.45μm有机相滤膜过滤,在Agela Promosil C_(18)色谱柱上进行分离,在柱温35℃条件下以不同体积比的0.2%(体积分数)甲酸溶液-乙腈混合溶液为流动相进行梯度洗脱,在波长290 nm处检测,记录色谱图。根据中药色谱指纹图谱相似度评价系统(2004版)建立了四块瓦的高效液相色谱(HPLC)指纹图谱,并采用IBM SPSS Statistics 25.0统计学软件和SIMCA软件(12.0版)进行主成分分析和偏最小二乘法判别分析。结果显示:11批四块瓦指纹图谱中有14个共有峰,与齐墩果酸对照品比对,确认12号峰对应齐墩果酸,11批四块瓦指纹图谱与对照指纹图谱的相似度为0.833~0.979;主成分分析共得到3个主成分,累计方差贡献率达到92.258%;偏最小二乘法判别分析筛选出影响不同产地四块瓦药材质量的8个差异性标志物。1 g of Sikuaiwa powder was taken and placed in the round bottom flask,and 50 mL of 75%(volume fraction,the same below)methanol solution was added.The mixture was reflux extracted for 1 h and filtered.The filtrate was made its volume up to 50 mL with 75%methanol solution,and passed through 0.45μm organic filter membrane.The test solution of Sikuaiwa was separated on Agela Promosil C_(18) column,using the mixed solution composed of 0.2%(volume fraction)formic acid solution and acetonitrile at different volume ratios as mobile phase for gradient elution at 35℃of column temperature.The components of the test solution were detected at wavelength of 290 nm,and the chromatogram was recorded.High performance liquid chromatography(HPLC)fingerprint of Sikuaiwa was established according to the Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(2004 Edition).The principal component analysis and partial leastsquare discriminant analysis were carried out by IBM SPSS Statistics 25.0 software and SIMCA software(12.0 Edition).As shown by the results,there were 14 common peaks in the fingerprints of 11 batches of Sikuaiwa.Compared with the oleanolic acid reference substance,the compound of peak 12 was confirmed to be oleanolic acid,and the similarity was in the range of 0.833-0.979 between fingerprints of 11 batches of Sikuaiwa and reference fingerprint.Three principal components were obtained by principal component analysis,and the cumulative variance contribution rate reached 92.258%.The 8 differential markers that affected the quality of Sikuaiwa from different origins were screened out by partial least-square discriminant analysis.

关 键 词：四块瓦 指纹图谱 高效液相色谱法 化学计量学 

分 类 号：O657.7[理学—分析化学]