State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Sciences, Health Science Centre, Peking University, Beijing, P. R. China.
J Sep Sci. 2011 May;34(10):1157-66. doi: 10.1002/jssc.201100022. Epub 2011 Apr 13.
In this study, the investigation of the volatile compounds of dried rhizomes of Coptis chinensis Franch, C. deltoidea C. Y. Cheng et Hsiao, and C. teeta Wall was carried out to complete the chemical composition of these valuable natural products. Volatile profiles were established and compared after headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm) fibre coupled to comprehensive 2D gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS). Analyses were performed and compared on two column-phase combinations (non-polar/polar and polar/non-polar). The majority of the identified compounds eluted as well-separated (pure) components as a result of high-resolution capability of the GC×GC method, which significantly reduces co-elution. Therefore, this increases the likelihood that pure mass spectra can be obtained. More than 290 volatile and semi-volatile organic compounds were tentatively characterized by means of GC×GC in tandem with TOFMS detection. Improved result interpretations were obtained in terms of compound classification based on the organized structure of the peaks of structurally related compounds in the GC×GC contour plot. These compounds are distributed over the chemical groups of hydrocarbons, acids, alkenes, alkynes, aldehydes, ketones, alcohols, esters, furans, and terpenoids. Among all the chemical groups, terpenoids present the higher number of identified compounds (44), alkenes (41), and aldehydes and ketones (28). This study completed the volatile phytochemical analysis of the headspace composition of various Coptis species rhizomes, and should serve as a means to identify the difference between the rhizomes and may also be useful to confirm individual species based on their volatile chemical profile.
本研究对黄连、三角叶黄连和云连的干燥根茎中的挥发性化合物进行了调查，以完成这些有价值的天然产物的化学成分研究。采用顶空固相微萃取（HS-SPME），使用聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB，65μm）纤维与二维气相色谱飞行时间质谱联用（GC×GC-TOFMS）建立并比较了挥发性图谱。在两种柱相组合（非极性/极性和极性/非极性）上进行了分析和比较。由于 GC×GC 方法的高分辨率能力，大多数鉴定出的化合物作为分离良好（纯）的组分洗脱，这显著减少了共洗脱。因此，这增加了获得纯质谱的可能性。通过 GC×GC 与 TOFMS 联用，共鉴定出 290 多种挥发性和半挥发性有机化合物。通过基于 GC×GC 等高线图中结构相关化合物峰的结构化组织对化合物进行分类，可以获得更好的结果解释。这些化合物分布在烃类、酸类、烯烃、炔烃、醛类、酮类、醇类、酯类、呋喃类和萜类等化学基团中。在所有的化学基团中，萜类化合物的鉴定数量最多（44 种），其次是烯烃（41 种）和醛类和酮类（28 种）。本研究完成了各种黄连属植物根茎顶空成分的挥发性植物化学分析，这不仅有助于识别根茎之间的差异，还可能有助于根据其挥发性化学特征来确认个别物种。
