檀香挥发油GC-MS指纹图谱研究

目的：建立檀香挥发油的指纹图谱分析方法，为檀香药材的质量评价提供方法与依据。方法：采用乙醚冷浸法提取檀香挥发油，应用GC-MS联用技术，采用HP-5弹性石英毛细管柱（30 m×0.32 mm，0.25 μm），程序升温（柱温90℃，以5℃·min^-1升至160℃，再以0.5℃·min^-1升至165℃，然后再以l℃·min^-1升至180℃，最后10℃·min^-1升至230℃），建立挥发油的共有峰指纹图谱，采用中南大学指纹图谱相似度评价软件和SPSS 20.0软件对不同来源的檀香油对照品及14批样品挥发油分别进行相似度评价和聚类分析。结果：所建立的檀香挥发油GC-MS指纹图谱有较好的重复性、精密度和稳定性（RSD均小于5%）。檀香油对照品及14批样品挥发油中α-檀香醇、β-檀香醇相对百分含量分别为34.225%~51.156%、20.897%~26.857%。以檀香油对照品为参照，14批样品挥发油相关系数为0.622~0.984，相合系数为0.628~0.984，但同一基地采集的5批檀香样品挥发油相关系数为0.924~0.984，相合系数为0.934~0.984，市购檀香样品挥发油相关系数为0.622~0.868，相合系数为0.628~0.838。通过聚类分析，在类间距离=15时，檀香油对照品及14批样品可以分为两类，檀香油对照品及S2~S9号样品为一类，S10~S15号样品为一类。结论：所建立的檀香挥发油GC-MS指纹图谱法为中药檀香的质量控制提供了一种有效手段。同一种植基地檀香样品的指纹图谱相似度较高，质量较均一；市售檀香样品的指纹图谱相似度较低，质量参差不齐。

Objective: To establish a fingerprint determination method of sandalwood essential oil, and provide a method and reference for quality control of sandalwood medicinal materials. Methods: Ether soaking method was used to extract volatile oil from sandalwood, and GC-MS technology was applied with an HP-5 fused silica capillary column(30 m×0.32 mm, 0.25 μm) and programmed temperature(column temperature was initially 90℃, and increased to 160℃ at the speed of 5℃·min^-1, then to 165℃ at the speed of 0.5℃·min^-1, further to 180℃ at the speed of l℃·min^-1, and at last to 230℃ at the speed of 10℃·min^-1) to establish the common peak fingerprint of volatile oil. Central South University fingerprint similarity evaluation software and SPSS 20.0 software were used to conduct similarity evaluation and cluster analysis for sandalwood oil reference substances from different sources and 14 batches of volatile oil samples. Results: The established GC-MS fingerprint for sandalwood essential oil had good repeatability, precision and stability(RSDs were less than 5%). The relative percentage contents of alpha-santalol, beta-santalol in 15 batches of essential oil were 34.225%-51.156% and 20.897%-26.857%, respectively. With sandalwood oil control products as reference, the correlation coefficients of 14 batches of volatile oil samples were 0.622-0.984,and their consistency coefficients were 0.628-0.984;the correlation coefficients of 5 batches of sandalwood essential oil samples from the same base were 0.924-0.984, and the consistency coefficients were 0.934-0.984;the correlation coefficients of purchased sandalwood essential oil samples were 0.622-0.868, and their consistency coefficients were 0.628-0.838. Through cluster analysis, when the intra-class distance was 15, the sandalwood oil reference substances and volatile oil samples could be divided into two categories-sandalwood oil reference substances and S2-S9 samples in the 14 batches of samples were integrated into one class of volatile oil, while S10-S15 samples in 14 batches of samples were integrated into the other class of volatile oil. Conclusion: The GC-MS fingerprint method established for sandalwood essential oil could provide an effective means for the quality control of traditional Chinese medicine(TCM) sandalwood. The similarity in fingerprint of sandal samples from the same planting base was higher, and the quality was more uniform;in contrast, the similarity in fingerprint of commercially available sandalwood samples was low, and the quality was uneven.