摘要
目的 建立化橘红药材的超高效液相色谱(UPLC)指纹图谱,并进行化学模式识别分析及含量测定,以鉴别不同基原的化橘红差异。方法 通过建立UPLC指纹图谱,确定20批化橘红样品共有峰及峰面积,采用《中药色谱指纹图谱相似度评价系统》(2012A版)进行相似度分析。以共有峰峰面积数据为基础,采用统计分析软件SPSS 19.0进行聚类分析,SIMCA 13.0进行主成分分析(PCA)及正交偏最小二乘法判别分析(OPLS-DA),并对指认的化学成分进行含量测定。结果 UPLC指纹图谱确定了18个共有峰,指认其中5、6、8、12、15号峰分别为7-羟基香豆素、柚皮苷、野漆树苷、佛手柑内酯、异欧前胡素;相似度评价结果显示样品S2、S3、S6、S8相似度介于0.851~0.891之间,其余16批样品相似度均>0.900。聚类分析可大致区分毛橘红和光橘红,少数批次存在偏差;PCA和OPLS-DA结果显示毛橘红和光橘红有更明显的区分趋势,并筛选出3个可能造成两种化橘红差异的标志物。含量测定结果表明,化橘红近成熟组柚皮苷含量高于幼果组和未成熟组(P<0.05),未成熟组佛手柑内酯含量明显高于近成熟组(P<0.05),各组野漆树苷、异欧前胡素含量无显著性差异。结论 所建立的UPLC指纹图谱结合化学模式识别及含量测定方法,可系统、全面地评价化橘红药材质量,筛选出的差异性标志物可为药效物质研究提供参考。
Objective To establish UPLC fingerprints of Citri Grandis Exocarpium from different origins,and then analyze the samples by combination of chemical pattern recognition and content determination. The aim of our study was to find the difference of Citri Grandis Exocarpium from different origins.MethodsThe UPLC fingerprints of 20 bathes of samples were established to confirm the common peaks and peak area. Similarity analysis was then performed using “Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine”(2012A Edition). Based on the common peak area data,cluster analysis was done by using SPSS 19.0,principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA)were carried out by using SIMCA 13.0. The content of the identified components was also determined.Results 18 common peaks were identified by UPLC fingerprint. We identified peak 5,6,8,12,15 as 7-hydroxycoumarin,naringin,rhoifolin,bergamot lactone,isoimperatorin,respectively. Similarity evaluation result displayed that the similarity of S2,S3,S6 and S8 was in the range of 0.851 to 0.891,the similarity of other 16 batches of samples was greater than 0.900.Cluster analysis can be used to roughly distinguish Citri grandis “Tomentosa” and Citrus grandis, but a small amount of them was inconsistent. The results of PCA and OPLLS-DA showed that there was obvious distinctive trend between Citri grandis “Tomentosa” and Citrus grandis. Furthermore, we selected 3 marking substance, which may be the cause of difference between two kinds of Citri Grandis Exocarpium. Content analysis indicated that naringin content of Citri Grandis Exocarpium in the near-mature group was higher than that in the young-fruit group and the immature group(P<0.05). The content of bergamot lactone in the immature group was higher than that in in the near-mature group(P<0.05). And there was no significant difference for content of rhoifolin and isoimperatorin among other groups.Conclusion We could evaluate quality of Citri Grandis Exocarpium comprehensively by means of UPLC fingerprints,chemical pattern recognition and content determination. The selected marking substance would provide reference for the research of effective substances.
作者
张靖年
胥爱丽
李养学
李素梅
陈昭
肖观林
ZHANG Jingnian;XU Aili;LI Yangxue;LI Sumei;CHEN Zhao;XIAO Guanlin(Guangdong Provincial Second Hospital of Traditional Chinese Medicine(Guangdong Provincial Engineering Technology Research Institute of Traditional Chinese Medicine)/Guangdong Provincial Key Laboratory of Research and Development in Traditional Chinese Medicine,Guangzhou 510095 Guangdong,China)
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2023年第1期103-109,共7页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
2021年省属科研机构稳定性支持项目(粤财科教[2021]113号)。
关键词
化橘红
超高效液相色谱指纹图谱
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
Citri Grandis Exocarpium
UPLC fingerprints
cluster analysis
principal component analysis
orthogonal partial least squares discriminant analysis
determination of content
