一测多评法结合Q型聚类分析对苍术中3个聚炔类成分的比较研究

Comparative study of three polyacetylenes in Atractylodis Rhizoma by QAMS combined with Q-type cluster analysis

目的:建立苍术药材中3个聚炔类挥发性成分[苍术素醇、(4E,6E,12E)-十四碳三烯-8,10-二炔-1,3-二乙酸酯(TDDA)、苍术素]的一测多评含量测定方法,并结合Q型聚类分析法对苍术中这3个成分进行分析,区分茅苍术与北苍术,为苍术药材质量控制提供依据。方法:将苍术素作为内参物,建立苍术素醇、TDDA与苍术素的相对校正因子,并计算二者含量;同时采用高效液相色谱外标法对上述3个聚炔类成分的含量进行测定,并比较两法的差异,以验证一测多评法的可行性和准确性。采用Q型聚类分析法对茅苍术与北苍术中上述3个聚炔类成分进行分析。结果:苍术素醇、TDDA、苍术素3个聚炔类成分在其各自范围内的线性关系良好(r≥0.9999),平均加样回收率为99.7%~101.9%,RSD为2.5%~3.7%,且在不同实验条件下重现性良好。22批苍术药材中,茅苍术与北苍术中苍术素含量范围分别为4.0659~5.4573、7.1417~8.5541 mg·g^-1,3个聚炔类成分含量总和的范围分别为5.6115~7.1828、9.9517~12.0745 mg·g^-1。一测多评的含量计算结果与HPLC外标法的测定结果无显著性差异(P>0.05)。采用Q型聚类分析法对测定结果进行分析,树状图显示茅苍术、北苍术药材各自聚为一类。结论:本文建立的一测多评法稳定且较可靠,Q型聚类分析法结合苍术中聚炔类成分的含量可较好地区分茅苍术与北苍术,为苍术药材的质量控制提供相关依据。

Objective:To establish a quantitative analysis of multi-components by single marker(QAMS)for the determination of three volatile polyacetylenes[atractylodinol,(4E,6E,12E)-tetradecatriene-8,10-diyne-1,3-diacetate(TDDA)and atractylodin]in Atractylodis Rhizoma.Combined with Q-type cluster analysis method,the three polyacetylenes components in Atractylodis Rhizoma were analyzed to distinguish A.lancea and A.chinensis,which provided a basis for the quality control of Atractylodis Rhizoma.Methods:The relative correction factors(RCFs)of atractylodinol and TDDA were determined by HPLC with atractylodin as the internal reference,which were used to calculate the contents of the two components.Meanwhile,external standard method by HPLC was used.The two methods were compared to validate the accuracy and feasibility of the new method.Q-type cluster analysis was used to analyze these three polyacetylenes components in A.lancea and A.chinensis.Results:These three polyacetylenes components showed good linear relationships within their respective ranges(r≥0.9999),whose average recoveries were 99.7%-101.9% with RSDs of 2.5%-3.7%.And repeatability under different experimental conditions was good.Among the 22 batches of Atractylodis Rhizoma,the contents of atractylodin in A.lancea and A.chinensis were 4.0659-5.4573 and 7.1417-8.5541 mg·g^-1,and the total contents of three polyacetylenes were 5.6115-7.1828 and 9.9517-12.0745 mg·g^-1 respectively.No significant difference was found in the quantitative results of the three components between the measured value and the calculated value(P>0.05).The results were analyzed by Q-type cluster analysis and the tree diagram showed that A.lancea and A.chinensis were clustered into two categories.Conclusion:The QAMS method established in this paper is feasible and accurate,and it can distinguish A.lancea and A.chinensis by Q-type cluster analysis combined with the contents of polyacetylenes in Atractylodis Rhizoma.This method can be applied in the quality control of Atractylodis Rhizoma.