基于热分析技术、指纹图谱及含量测定的不同产地酒黄芩质量评价

Quality Evaluation of Wine-processed Scutellariae Radix from Different Origins Based on Thermal Analysis Technology,Fingerprint and Content Determination

目的:利用热分析技术探讨黄芩和酒黄芩饮片的热解温度范围,采用指纹图谱和指标成分含量测定比较不同产地酒黄芩的质量差异,为酒黄芩生产工艺及质量评价提供依据。方法:采用热分析技术,对生黄芩饮片、酒黄芩饮片、黄芩浸出物,以及主要成分黄芩苷、黄芩素、汉黄芩苷、汉黄芩素的热解特性进行分析,确定酒黄芩最佳炮制温度范围,并结合层次分析法(AHP)、指标相关性的指标权重确定法(CRITIC)及加权评价法优选最佳炮制时间。按优选条件对山西、河北及甘肃3个产地的黄芩饮片进行炮制,采用超高效液相色谱法(UPLC)建立酒黄芩指纹图谱,并对指纹图谱进行相似度分析及共有峰指认;同时,对黄芩苷、白杨素-7-O-葡萄糖醛酸苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A的含量进行检测,比较不同产地生黄芩、酒黄芩的质量差异。基于7种指标成分含量进行聚类分析(HCA)、主成分分析(PCA)及正交偏最小二乘法-判别分析(OPLS-DA),以变量重要性投影(VIP)值>1筛选酒黄芩组间差异性成分。结果:酒黄芩的最佳炮制温度为190~200℃,优选酒炙工艺为190℃炒制8 min。不同产地生黄芩指纹图谱与对照图谱的相似度均≥0.97,酒黄芩指纹图谱与对照图谱的相似度均≥0.98,提示炮制可在一定程度上使饮片质量趋于一致。含量测定结果显示,甘肃产黄芩中苷类成分含量相对另外2个产地样品较低,而苷元类成分含量较高;各产地黄芩经酒炙后7种指标成分含量整体略呈降低趋势,以甘肃产地样品的含量降低幅度较大;多元统计分析及判别分析结果表明,汉黄芩苷是区分不同产地酒黄芩的关键成分。结论:该研究确定了酒黄芩炮制的最佳工艺,并筛选出产地间差异性成分汉黄芩苷,可为酒黄芩质量评价提供参考依据。

Objective:The pyrolysis temperature range of Scutellariae Radix(SR)and wine-processed SR(WSR)was studied by thermal analysis technique,and the quality difference in the contents of main components and fingerprint of WSR from different producing areas was compared,in order to provide a basis for the production process and quality evaluation of WSR.Method:Thermal analysis technology was used to analyze the pyrolysis properties of SR,WSR,extract of SR and main components(baicalin,baicalein,wogonoside and wogonin),so as to determine the optimal processing temperature range of WSR.Then combined analytic hierarchy process(AHP),criteria importance through intercrieria correlation(CRITIC)and weighting evaluation,the optimal processing time was optimized.Based on the optimal conditions,SR from Shanxi,Hebei and Gansu provinces were processed.Ultra performance liquid chromatography(UPLC)was employed to establish the fingerprint of WSR,and the similarity analysis and common peak identification were carried out.At the same time,the contents of seven representative components(baicalin,chrysin-7-Oglucuronide,oroxylin A-7-O-β-D-glucuronide,wogonoside,baicalein,wogonin and oroxylin)were determined,then the quality differences of SR and WSR from different origins were compared.Based on the contents of seven active components,different batches of WSR were classified by hierarchical cluster analysis(HCA),principal component analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLSDA),the variable importance in the projection(VIP)value>1 was used to screen the differential components of each group.Result:The optimum processing temperature of WSR was 190-200℃,and 190℃ for 8 min was selected as the frying process.The similarities between the fingerprints of SR and their control fingerprint were≥0.97,and the similarities between the fingerprints of WSR and their control fingerprint were≥0.98,suggesting that the processing could make the quality of decoction pieces consistent to a certain extent.The content determination results showed that the content of glycosides in SR from Gansu was lower than that from the other 2 producing areas,but the content of aglycones was higher.After being processed with wine,the content of 7 index components in SR from all producing areas decreased slightly,and the content of sample from Gansu province decreased greatly.The results of multivariate statistical analysis and discriminant analysis showed that wogonoside was the key ingredient for distinguishing WSR from different producing areas.Conclusion:This study determined the best processing technology of WSR and screened out the different component of wogonoside to distinguish between different origins of WSR,which can provide reference for the quality evaluation of WSR.