包尔胡特果实的化学成分分析及综合质量评价

Analysis of chemical constituents and comprehensive quality evaluation of Rhamni Songoricae Fructus

目的 鉴定包尔胡特果实的化学成分,并建立其指纹图谱和同时测定4种成分含量的方法,以综合评价包尔胡特果实的质量。方法 采用超高效液相色谱四极杆-飞行时间串联质谱法鉴定包尔胡特果实中的化学成分。采用高效液相色谱(HPLC)法建立15批包尔胡特果实(编号S1~S15)的指纹图谱,并采用SPSS 26.0与SIMCA 14.1软件进行化学计量学分析;同法测定槲皮素、山柰酚、山柰素、大黄素的含量。结果 包尔胡特果实中共鉴定出35种化合物,包括28种黄酮类成分、5种蒽醌类成分、2种有机酸类成分;其HPLC指纹图谱中共标定19个共有峰,指认出槲皮素、山柰酚、山柰素和大黄素;15批样品的HPLC指纹图谱与对照指纹图谱的相似度均大于0.9。聚类分析结果显示,15批样品聚为2类,其中S1~S5、S7、S9为一类,其余样品为一类,与主成分分析结果相同;正交偏最小二乘法-判别分析结果显示,2、6、1、11(槲皮素)、3、14、8、10、19(大黄素)、5号峰的变量重要性投影值均大于1。槲皮素、山柰酚、山柰素、大黄素的含量分别为0.710~10.478、0.236~0.660、0.334~3.039、0.261~0.504 mg/g。结论 所建化学成分鉴定方法、指纹图谱和含量测定方法简便可行、重复性好,结合化学计量学分析可用于包尔胡特果实质量的综合评价。

OBJECTIVE To identify the chemical constituents of Rhamni Songoricae Fructus and to establish their fingerprints and the method for simultaneous determination of four constituents to comprehensively evaluate the quality of Rhamni Songoricae Fructus.METHODS The chemical constituents in Rhamni Songoricae Fructus were qualitatively analyzed by ultra-performance liquid chromatography quadrupole-time-of-flight tandem mass spectrometry.The fingerprints of 15 batches of Rhamni Songoricae Fructus were established by HPLC and chemometric analysis was performed by using SPSS 26.0 and SIMCA 14.1 software;the contents of quercetin,kaempferol,kaempferide and emodin were determined by the same method.RESULTS A total of 35constituents were identified,including 28 kinds of flavonoids,5 kinds of anthraquinones and 2 kinds of organic acids.A total of 19common peaks were identified in the HPLC fingerprints,recognizing quercetin,kaempferol,kaempferide and emodin.The similarities between HPLC fingerprints of 15 batches of samples and control chromatograms were greater than 0.9.The results of cluster analysis showed that 15 batches of samples were divided into 2 classes,of which S1-S5,S7 and S9 were one class and the rest were one class,similar to the results of principal component analysis.The results of the orthogonal partial least squaresdiscriminant analysis showed that the variable importance projections of peaks No.2,6,1,11(quercetin),3,14,8,10,19(emodin),5 were all greater than 1.The contents of quercetin,kaempferol,kaempferide and emodin ranged from 0.710 to 10.478mg/g,0.236 to 0.660 mg/g,0.334 to 3.039 mg/g,and 0.261 to 0.504 mg/g.CONCLUSIONS The constructed chemical constituent identification,fingerprint and content determination methods are simple,feasible and reproducible,which combined with chemometric analysis can be used for comprehensive evaluation of the quality of Rhamni Songoricae Fructus.