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不同淫羊藿羊脂油烘制品的HPLC指纹图谱建立、多元统计分析及烘制工艺优化
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篇名: 不同淫羊藿羊脂油烘制品的HPLC指纹图谱建立、多元统计分析及烘制工艺优化
TITLE: Establishment of HPLC Fingerprint ,Multivariate Statistical Analysis and Processing Technology of Different Suet Oil-baked Epimedium brevicornum
摘要: 目的:建立不同淫羊藿羊脂油烘制品的高效液相色谱(HPLC)指纹图谱,并筛选最优烘制工艺。方法:采用HPLC法。以淫羊藿苷为参照,绘制22批样品的HPLC指纹图谱,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价,确定共有峰。采用SIMCA14.1统计App进行聚类分析(HCA)、主成分分析(PCA)、正交偏最小二乘法-判别分析(OPLS-DA),以变量投影重要性值大于1为标准,筛选影响淫羊藿羊脂油烘制品质量的差异标志物,并以其为指标经烘制动力学研究筛选烘制工艺。结果:22批样品共有18个共有峰,相似度为0.831~0.991;共指认朝藿定A、朝藿定B、朝藿定C、淫羊藿苷、箭藿苷A、箭藿苷B、宝藿苷Ⅰ等7个共有峰。22批样品可聚为两类,S19~S22为Ⅰ类,S1~S18为Ⅱ类;其中Ⅱ类又可聚为Ⅱa(S15~S18)、Ⅱb(S10~S14)、Ⅱc(S1~S9)等3类;PCA结果与上述结果一致。OPLS-DA结果显示,淫羊藿苷、箭藿苷B、宝藿苷Ⅰ为影响淫羊藿羊脂油烘制质量的差异标志物。动力学研究结果显示,淫羊藿苷在180℃烘制25min或190℃烘制20min,宝藿苷Ⅰ在180℃烘制30min或190℃烘制15min,箭藿苷B在210℃烘制18min时含量达到最高,根据上述结果最终确定最优烘制工艺为180℃烘制25~30min或190℃烘制15~20min。结论:所建指纹图谱方法稳定、可靠,重复性好,多元统计分析可用于反映淫羊藿在不同烘制条件下化学成分的变化情况及初步筛选烘制工艺。
ABSTRACT: OBJECTIVE:To establish HPLC fingerprint of different products of suet oil-baked Epimedium brevicornum ,and to screen the optimal baking technology. METHODS :HPLC method was adopted. Using icariin as reference ,HPLC fingerprints of 22 batches of samples were drawn. The similarity was evaluated by using Similarity Evaluation System of TCM Chromatographic Fingerprint(2012 edition),and common peaks were confirmed. HCA ,PCA and OPLS-DA analysis were performed by SIMCA 14.1 statistical software. Taking variable importance in the project >1 as criteria ,biomarkers affecting the quality difference of suet oil-baked E. brevicornum were screened ;using mass marker as index ,the baking technology was screened by baking technology. RESULTS:There were 18 common peaks in 22 batches of samples. The similarities were between 0.831 and 0.991. Totally 7 common peaks were identified ,i.e. epimedin A ,epimedin B ,epimedin C ,icariin,sagittatoside A ,sagittatoside B ,baohuoside Ⅰ. The 22 batches of samples were clustered into two categories ,S19-S22 were clustered into category Ⅰ and S 1-S18 were clustered into category Ⅱ. The category Ⅱ was sub-clustered into category Ⅱa(S15-S18),category Ⅱb(S10-S14),category Ⅱc (S1-S9);the result of PCA analysis was consistent with above results. OPLS-DA showed that the biomarkers affecting the quality difference were icariin ,sagittatoside B and baohuoside Ⅰ. The results of kinetic studies showed that the content of icariin when baked at 180 ℃ for 25 min or 190 ℃ for 20 min,that of baohuoside Ⅰ when baked at 180 ℃ for 30 min or 190 ℃ for 15 min and that of epimedin B when baked at 210 ℃ for 18 min were the highest ;according to above results ,the optimal baking technology was baking at 180 ℃ for 25-30 min or 190 ℃ for 15-20 min. CONCLUSIONS :Established fingerprint is stable , reliable and reproducible. The multivariate statistical analysis can be used for the changes of chemical components in E. brevicornum under different baking condition and preliminary selection of baking technology.
期刊: 2020年第31卷第12期
编辑: 李园,李秀丽,王淑,王信,曹广尚,孙萍,郭功玲
AUTHORS: LI Yuan,LI Xiuli,WANG Shu,WANG Xin,CAO Guangshang,SUN Ping,GUO Gongling
关键字: 淫羊藿;羊脂油烘制;高效液相色谱法;指纹图谱;多元统计分析;烘制工艺优化
KEYWORDS: Epimedium brevicornum ;Suet oil-based ;HPLC;Fingerprint;Multivariate statistical analysis ;Optimization of
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