HS-GC-MS结合化学计量学方法快速鉴别木香及其纸煨品的实验研究

目的：建立一种通过快速分析挥发性成分来区别木香及其炮制品木香纸煨品的方法。方法：在优化药材粒度、顶空加热温度和顶空平衡时间等提取条件的基础上，建立了木香的顶空进样结合气相色谱联用质谱法（HS-GC-MS），并以水杨酸甲酯为内标，使用保留指数结合质谱库对化合物进行定性，在此基础上采用主成分分析（PCA）和偏最小二乘判别分析（PLS-DA）方法对HS-GC-MS的结果进行评价。结果：最佳顶空提取条件为：药材打粉过3号筛，顶空加热温度90℃，平衡时间40 min。利用建立的HS-GC-MS方法并结合保留指数从木香及其炮制品中鉴定出了33个共有成分（包括17个已确定化合物及16个未知成分），通过化学计量学方法对HS-GC-MS数据进行处理，实现了木香及其炮制品的鉴别，并寻找到了区分木香及其炮制品木香纸煨品的特征挥发性成分，分别为愈创木基-1（10），11-二烯和β-榄香烯。结论：HS-GC-MS结合化学计量学的方法快速简单，可用于鉴别木香与煨木香。

Objective: To establish a rapid method for the discrimination of Aucklandiae Radix and its roasted products with the analysis of volatile components.Methods: On the basis of optimizing extraction conditions such as particle size,headspace heating temperature and headspace equilibrium time,a method for detecting Aucklandiae Radix by headspace sampling and gas chromatography-mass spectrometry(HS-GC-MS)was established.With methyl salicylate as internal standard,and retention indices coupled with MS library retrieval as qualitative method,the data of HS-GC-MS was analysed by partial least squares discriminant analysis(PLS-DA) and principal component analysis(PCA)further.Results: The results of the orthogonal experiments showed the optimum headspace conditions were as follows:The medicinal materials were crushed through sieve 3,heated at 90℃ and balanced for 40 min.Thirty-three common compounds,including seventeen determined compounds and sixteen unknown compounds,were identified from Aucklandiae Radix and its processed products by the established HS-GC-MS method coupled with retention indices.Then the raw Aucklandiae Radix and its roasted products were distinguished by chemometrics analysis based on the HS-GC-MS data.The characteristic volatile components of Aucklandiae Radix were also found as guaia-1(10)and 11-diene and β-elemene.Conclusion: The HS-GC-MS combined with chemometrics analysis can be used as a simple and rapid method to discriminate the Aucklandiae Radix and its roasted products.

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