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采用顶空气相色谱-质谱技术对不同产地莪术进行快速鉴别
吕狄亚,曹岩,董昕,李玲,娄子洋*,柴逸峰*
0
(第二军医大学药学院药物分析学教研室,上海市药物(中药)代谢产物研究重点实验室,上海200433
共同第一作者
*通信作者)
摘要:
目的 运用顶空气相色谱-质谱(HS-GC/MS)结合化学计量学方法对不同产地莪术进行鉴别,以便莪术的质量控制研究。方法 采用HP-5石英毛细管色谱柱(30 m×0.32 mm, 0.25 μm),进样口温度250℃,柱初始温度为50℃,保持3 min,以20℃/min升至150℃,最后以2℃/min升至200℃,保持10 min,分流比101。载气为氦气,流速:1.0 mL/min。顶空瓶区域温度:90℃;样品瓶加热平衡时间:30 min;进样量:1.5 mL。结合主成分分析和聚类分析方法对数据进行分析。结果 在15个批次的样品的图谱中选取18个共有色谱峰进行鉴定,采用主成分分析法能够有效地区分四川、广西和云南等不同产地的莪术药材,并明确了对药材造成差异的主要成分为β-榄香烯、莰烯、β-蒎烯、p-menth-1-en-8-ol、桉叶素、8,9-去氢-9-甲酰基-环异长叶烯。结论 应用HS-GC/MS技术与化学计量学方法相结合,建立了鉴别区分不同产地来源的莪术药材的方法,并找到了莪术中对分类起主要作用的特征性成分。
关键词:  莪术  顶空气相色谱-质谱法  主成分分析  聚类分析
DOI:10.3724/SP.J.1008.2013.00190
投稿时间:2012-10-25修订日期:2012-12-14
基金项目:国家自然科学基金(81273472).
Headspace GC-MS for fast identification of Rhizoma curcuma of different origins
Lü Di-ya,CAO Yan,DONG Xin,LI Ling,LOU Zi-yang*,CHAI Yi-feng*
(Department of Pharmaceutical Analysis, Shanghai Key Laboratory for Pharmaceutical (Chinese Materia Medica) Metabolite Research,School of Pharmacy, Second Military Medical University, Shanghai 200433, China
Co-first authors.
*Corresponding authors.)
Abstract:
Objective To distinguish Rhizoma curcuma of different origins using headspace-gas chromatography/mass spectrometry (HS-GC/MS) combined with principal components analysis (PCA) and hierarchical cluster analysis (HCA), so as to help the quality control of Rhizoma curcuma. Methods HP-5 capillary column (30 m×0.32 mm, 0.25 μm) was used under the following condition: inlet temperature: 250℃, initial column temperature: 50℃ maintained for 3 min, then increasing to 150℃ at 20℃/min and to 200℃ at 2℃/min, maintained for 10 min, with the split ratio being 101. The carrier gas was helium, with flow rate being 1.0 mL/min, hadspace vials regional temperature being 90℃, vials heating equilibration time being 30 min, and injection volume being 1.5 mL. The effect of extract separation conditions, temperature of the vial and equilibrium time on the extraction volatile components of Rhizoma curcuma were observed. Results PCA could distinguish 18 common peaks of 15 batches of Rhizoma curcuma from Sichuan, Guangxi and Yunnan, and it was confirmed that β-elemene, camphene, β-pinene, p-menth-1-en-8-ol, eucalyptol, and cycloisolongifolene, 8,9-dehydro-9-formyl were the main components to cause differences in Rhizoma curcuma of different origins. Conclusion We have established a method combining HS-GC/MS with PCA and HCA to distinguish Rhizoma curcuma of different origins, and we have also identified the major characteristic components of Rhizoma curcuma of different origins.
Key words:  Rhizoma curcuma  headspace-gas chromatography-mass spectrometry  principal component analysis  hierarchical cluster analysis