GC-MS分析郁金水蒸气蒸馏提取物和超临界提取物  被引量:5

Analysis of water vapor distillation extracts and supercritical fluid extracts of C.wenyujin with gas chromatography-mass spectrometry

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作  者:陈湘[1] 周明哲[1] 王嗣岑[1] 窦建卫[1] 

机构地区:[1]西安交通大学医学院,西安710061

出  处:《药物分析杂志》2007年第12期1932-1937,共6页Chinese Journal of Pharmaceutical Analysis

基  金:西安市科技局工业攻关项目(No.GG06077)

摘  要:目的:对郁金水蒸气蒸馏提取物和超临界提取物进行分析。方法:采用中国药典(2005年版)挥发油测定法和超临界二氧化碳流体萃取法(SFE—CO_2)对药用植物郁金进行提取。利用气相色谱-质谱联用技术(GC-MS)对提取物中的化学成分进行了分离分析,并采用峰面积归一化法计算各成分相对百分含量。GC-MS 分析采用 Rtx-5MS 毛细管色谱柱(30 mm×0.25 mm×0.25 μm)。进样口温度为280 ℃。程序升温,起始温度为140℃,以5℃·min^(-1)的升温速率升温至220℃,再以20℃·min^(-1)的升温速率升温至280 ℃,停留1 min。载气为氦气,流速为82.4 mL·min^(-1)。质谱中轰击电压为70 eV。离子源温度为200 ℃。全离子扫描,扫描范围为 m/z 40~500。结果:对郁金水蒸气蒸馏提取物的47种化学成分进行了鉴定,所鉴定的成分占总流出峰面积的96.1%;对郁金超临界萃取物的39种化学成分进行了鉴定,所鉴定的成分占总流出峰面积的86.8%。结论:实验结果为了解郁金的化学物质基础和进一步开发研究提供了依据。Objective:Analyze the constituents in water vapor distillation extraction and supercritical fluid CO2 extraction( SFE -CO2 ) of C. wenyufin. Methods: C. wenyujin was extracted with water vapor distillation and SFE - CO2 respectively,and analyzed by GC -MS. The GC -MS analysis with a Rtx-5MS capillary column (30 mm ×0. 25 mm,0. 25 μm film thickness) was used. The inlet temperature was maintained at 280 ℃. The column oven was begun at 140 ℃, then programmed from 140 to 220 ℃ at 5 ℃. min^-1, then programmed from 220 ℃ to 280 ℃ at 20 ℃. min ^- 1 and finally, held for 1 min. Helium at a constant flow rate of 82. 4 mL . min^ -1 was used as the carrier gas. The mass spectrometry conditions were as follows : ionization energy ,70eV ; ion source temperature ,200 ℃. The mass selective detectorwas operated in the TIC mode ( m/z 40 - 500). Results:For the analysis of the water vapor distillation extractions of C. wenyujin 47 peaks were separated and identified, the compounds were quantitatively determined by normalization method, and the identified compounds represent 96. 1% of total GC peak areas. For the analysis of the SFE -CO2 extractions of C. wenyufin 39 peaks were separated and identified,the compounds were quantitatively determined by normalization method, and the identified compounds represent 86. 8% of total GC peak areas. Conclusion:The results will provide important foundation for understanding the constituents and further exploitation of C. wenyujin.

关 键 词:郁金 水蒸气蒸馏法 超临界二氧化碳流体萃取法 气相色谱-质谱联用 

分 类 号:R917[医药卫生—药物分析学]

 

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