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白芷、川芎药对配伍挥发油成分的GC-MS分析
胡志妍1,2,齐天2,3,杨光2,杨旦2,4,付恩桃1,2,范国荣1,2*
0
(1. 福建中医药大学药学院药物制剂教研室, 福州 350108;
2. 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;
3. 安徽中医药大学药学院生药学教研室, 合肥 230038;
4. 上海海洋大学食品学院海洋生物资源利用研究室, 上海 201306
*通信作者)
摘要:
目的 研究白芷、川芎单味药及其药对的挥发油成分,并考察白芷、川芎药对配伍对挥发油成分的影响。方法 采用水蒸气蒸馏法提取白芷、川芎单味药及其药对的挥发油,运用气相色谱-质谱联用技术,结合计算机检索,并与文献资料比对,进行化学成分的分离和鉴定。色谱条件:TR5-MS毛细管色谱柱(30 m× 0.25 mm,0.25 μm);载气为高纯氦气;进样口温度250℃;进样量1 μL,分流比50:1;恒流模式,载气流速1.00 mL/min;程序升温:起始温度50℃,保持1 min,以5℃/min 的速率升至240℃,保持1 min,然后以5℃/min 升至280℃,并保持1 min。质谱条件:电子轰击(EI)离子源,电子能量70 eV,离子源温度220℃,传输线温度280℃,质量范围(m/z):50~650 amu,数据采集扫描模式为全扫描,溶剂延迟5 min。结果 在白芷、川芎、药对(1:1)、药对(4:1)的挥发油及白芷、川芎等浓度挥发油混合物(药对等浓度挥发油)中分别鉴定出69、59 、59、60、78 种化合物,其中共有成分19种。结论 从挥发油的组分及含量来看,不同配伍比例药对挥发油的成分有很大的不同,单味药挥发油组分的含量在药对中都发生了变化。
关键词:  白芷  川芎  药对  挥发油类  气相色谱-质谱法
DOI:10.3724/SP.J.1008.2014.00177
投稿时间:2013-08-11修订日期:2013-12-12
基金项目:国家自然科学基金(81273473).
GC-MS in analysis of chemical constituents of volatile oils in drug pair of Radix Angelica dahurica and Ligusticum chuanxiong Hort.
HU Zhi-yan1,2,QI Tian2,3,YANG Guang2,YANG Dan2,4,FU En-tao1,2,FAN Guo-rong1,2*
(1. Department of Pharmaceutics, School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350108, Fujian, China;
2. Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai Key Laboratory for Pharmaceutical (Chinese Materia Medica) Metabolite Research, Shanghai 200433, China;
3. Department of Pharmacognosy, School of Pharmacy, Anhui University of Traditional Chinese Medicine, Hefei 230038, Anhui, China;
4. Research Institute of Marine Bioresources Utilization, College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China
*Corresponding author.)
Abstract:
Objective To study the essential oil components in herbal pair (HP) of Radix Angelica dahurica-Ligusticum chuanxiong Hort.(RAD-LCH) and its single herb, and to investigate the influence of HP on the components of the volatile oil. Methods Essential oil was extracted from Radix Angelica dahurica and Ligusticum chuanxiong Hort. by steam distillation. Identification of extracted components was accomplished using GC-MS technique combined with library searching and literature comparison. Chromatography analysis was carried out on a TR5-MS capillary column (30 m× 0.25 mm, 0.25 μm); the carrier gas was high-purity helium; the inlet temperature was 250℃; the injection volume was 1 μL, the split ratio 501; constant current mode, the flow rate of carrier gas was 1.00 mL/min; the temperature program was as follows: 50℃ for one minute, rose to 240℃ at 5℃/min and maintained for one minute, then rose to 280℃ at 5℃/min and maintained for one minute. MS condition was as follows: electron impact (EI) ion source, electron energy 70 eV, ion source temperature 200℃, transmission line temperature 280℃, mass scan range m/z:50-650 amu, data acquisition scan mode for full scan, and solvent delay five minutes. Results There were 69, 59, 59, 60 and 78 volatile constituents in RAD, LCH, HP (1:1), HP (4:1) and essential oil of mixture of equal concentration from RAD and LCH (EOEC), and 19 common volatile components were identified. Conclusion Regarding the volatile oil constituents and content, the volatile oil compositions of different HP proportions vary greatly, accompanied by changed contents of volatile oil components of single herb in HP.
Key words:  Angelica dahurica  Ligusticum chuanxiong  paired drugs  volatile oils  gas chromatography-mass spectrometry