GC-MS分析比较人参花水蒸气与超临界CO2提取物及其脂肪酸成分的研究  

Comparative analysis on volatile oil extracted by steam distillation and supercritical fluid extraction carbon dioxide of Panax ginseng flower and its fatty acid identification using GC-MS approach

作　　者：王恩鹏[1] 陈雪[1] 孙岩[1] 张洪长[1] 刘淑莹[1] 陈长宝[1] WANG En-peng CHEN Xue SUN Yan ZHANG Hong-chang LIU Shu-ying CHEN Chang-bao(Changchun University of Traditional Chinese Medicine, Jilin Ginseng Academy, Changchun 130117, China)

机构地区：[1]长春中医药大学,吉林省人参科学研究院,长春130117

出　　处：《药物分析杂志》2016年第12期2153-2162,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：吉林省教育厅“十二五”科学技术研究项目(20150344);长春市科技局重大科技攻关项目(14KG057)

摘　　要：目的:对水蒸气蒸馏法(SD法)、超临界CO_2萃取法(SFECD法)提取的人参花挥发性成分进行分析比较,并鉴定人参花中的脂肪酸成分。方法:利用气相色谱-质谱联用技术(GC-MS技术)检测提取物及酸催化的人参花脂肪酸衍生物。色谱条件:采用HP-5ms(30 mm×0.25 mm×0.25μm)石英毛细管柱,载气为氦气,流速为1 m L·min^(-1),汽化室温度280℃,进样方式为分流进样,分流比为50∶1(挥发油)及30∶1(脂肪酸衍生物),进样量为1μL,溶剂延迟时间为3.8 min;检测以SD法提取的挥发油,以SFECD法提取的挥发油,以及脂肪酸衍生物时的柱温采用不同的升温程序。质谱条件:电离源为EI源,电离能量为70 e V,离子源温度230℃,四极杆温度150℃,加速电压1 300 V,质量扫描范围为m/z 50~550。以峰面积归一化法测得挥发油各组分相对百分含量。结果:通过与数据库及文献比对,鉴定出以SD法提取的挥发油中的67种成分,以SFECD法提取的挥发油中的20种成分,以峰面积归一化法计算上述2种提取方法提取的各组分相对百分含量分别占挥发油总流出物峰面积的89.67%及61.84%。水蒸气法提取人参花挥发油组分中含量超过1%的共有11个,全部为萜类;SFECD法提取人参花挥发油流出物中,含量在1%以上的有9个化合物,经酸催化衍生后鉴定出13种脂肪酸,主要为亚油酸、十四甲基-十五酸、亚麻酸,棕榈酸。结论:水蒸气蒸馏法提取的挥发油中低沸点,高挥发性组分含量较多,而超临界CO_2萃取法可萃取出较高的极性、高沸点组分,表明超临界法提取的挥发油分解情况较少,稳定性更好。Objective： To comparatively analyze the volatile of Panax ginseng flower extracted using the steam distillation （SD）extraction and supercritical fluid extraction carbon dioxide （SFECD）methods, and determine the fatty acid components.Methods： GC-MS was applied to test the extracts and the acid-catalyzed derivative of the fatty acid in Panax ginseng flower.A HP-5ms （30 mm×0.25 mm×0.25 μm）quartz capillary chromatographic column was employed during the analysis procedure, and relative percentage content of each component was calculated by area normalization method.The operating conditions were as follows：helium was used as a carrier gas at a flow rate of 1 mL·min-1, and injector temperature was 280℃.The samples were injected into GC by split mode with a split ratio of 50：1, with injection volume of each sample 1 μL, and the solvent delay time 3.8 min.Different heating programs were employed for essential oil and fatty acid derivatives.GC-MS analyses were performed in EI mode （70 eV）.The ion source temperature was 230℃, the quadrupole rods temperature was 150℃, the accelerated voltage was 1 300 V, and the mass scan range was m/z 50-550.Results： Based on the database and literature, 67 and 20 components of the extracts were respectively identified, and the relative content of each peak was detected by the normalization method of peak area.The total effluent areas are 89.67% and 61.84% respectively by SD and SFECD method according to the area normalization method.By SD method, the percentages of 11 components in the volatile oil were above 1%, and these components were all ascribed to terpenoid compounds.By SFECD method, the percentages of 9 components in the volatile oil were above 1%.13 components of the fatty acid were identified after the acid-catalyzation, which were mainly ascribed to linoleic acid, Methyl 14-methylpentadecanoate, linolenic acid and palm acid.Conclusion： There were more components with low boiling point and high volatility in the extracts prepared by SD metho

关 键 词：人参花 挥发油 水蒸气 超临界C02萃取 脂肪酸 亚油酸 十四甲基-十五酸 亚麻酸 棕榈酸 气相色谱-质谱(GC-MS) 

分 类 号：R917[医药卫生—药物分析学]