苦石莲皮普通粉和微粉挥发性成分对比研究.doc

苦石莲皮普通粉和微粉挥发性成分对比研究 作者：袁月玲 霍昕 高玉琼 刘莹 丁丽娜 杨迺嘉【摘要】 目的研究苦石莲皮中的挥发性成分，并对比普通粉和微粉中挥发性成分异同。方法利用有机溶剂水蒸气蒸馏法提取苦石莲皮中的挥发成分，用气相色谱质谱联用（GC-MS）进行测定，色谱柱为HP-5MS 5% Phenyl Methyl Siloxane弹性石英毛细管柱(30 m0.25 mm0.25 m)，结合计算机检索技术对分离的化合物进行结构鉴定，应用色谱峰面积归一化法计算各成分的相对百分含量。结果苦石莲皮普通粉中分离出115个化学成分，鉴定出63个化学成分，检出率为54.7，其中相对百分含量大于2.0有5种；微粉中分离出119个化学成分，鉴定出64个化学成分，检出率为53.7，其中相对百分含量大于2.0有9种。两种粉末挥发性成分中有54种相同成分，微粉中含量高于普通粉中相应成分的有28种，其中含量最高的分别是柠檬烯（5.311%，普通粉）和亚油酸甲酯（3.388微粉）。结论该实验首次对苦石莲皮普通粉和微粉挥发性成分进行对比研究。 【关键词】 苦石莲； 有机溶剂水蒸气蒸馏； 挥发性成分； 气相色谱-质谱联用Abstract：ObjectiveTo study the chemical constituents of volatile constituents from the shell of Caesalpinia minax Hance. MethodsThe chemical compositions of the volatile constituents of the plant which were obtained by extraction with water added by residual solvent were analyzed by GC-MS equipped with a elastic quartz capillary column-HP-5MS 5% Phenyl Methyl Siloxane (30 m0.25 mm0.25 m). The constituents were identified by their mass spectra. The relative percentage of the volatile constituents was calculated from the GC peak areas.ResultsOne hundred and fifteen kinds of chemical constituents from the ordinary powder of the shell of Caesalpinia minax Hance were separated and sixty-three of them, which accounts for 54.7%, were characterized. There were five kinds whose relative contents were more than 2.0%; One hundred and nineteen kinds of chemical constituents from the micronized powder of the shell of Caesalpinia minax Hance were separated and sixty-four of them, which accounted for 53.7% , were characterized. There were nine kinds whose relative contents were more than 2.0%; There were the same of fifty-four kinds chemical constituents in the two kinds of powder, of which the contents of twenty-eight constituents from the micronized powder were more than those in the ordinary powder. The most relative contents were Limonene(5.311% ordinary powder) and Methyl linoleate(3.388%, micronized powder ) . ConclusionThis paper reports, for the first time, the comparison of volatile constituents of both the ordinary and micronized powder of the shell of Caesalpinia minax Hance.Key words：Caesalpinia minax Hance; Extract with water added by residual solvent; Volatile constituents; GC-MS 苦石莲来源于豆科植物喙荚云实Caesalpinia minax Hance的成熟种子。喙荚云实生于海拔2001 800 m的次生林缘、灌木丛中，分布于广东、海南、广西、贵州和云南等地1，是傣族的民族用药。苦石莲味苦，性凉，功能清火解毒，杀虫止痒，消肿止痛；用于治疗乳痈、蜈蚣咬伤及疔疮痈疖脓肿等1。国内外仅对其鉴别2及药用考证3研究有报道，未见对其挥发性成分的研究。本实验采用有机溶剂水蒸气蒸馏法从苦石莲皮的普通粉和微粉中提取出挥发性成分，并用气相色谱-质谱-计算机联用系统对苦石莲皮的普通粉和微粉中挥发性成分进行定性定量的对比研究，为深度开发该民族用药以及为其质量控制提供必要的基础数据。1 仪器与材料1.1 仪器 挥发油提取器和美国惠普公司HP-6890/HP5973 GC-MS气质联用仪。HP-5MS5% Phenyl Methyl Siloxane弹性石英毛细管柱(30 m0.25 mm0.25 m)。1.2 试剂与材料 蒸馏水和无水硫酸钠（国产分析纯试剂）。药材：苦石莲皮(80目)、苦石莲皮（200目）(为同一批次苦石莲药材的皮，苦石莲产自贵州，由贵阳中医学院孙庆文老师鉴定为豆科植物喙荚云实Caesalpinia minax Hance的成熟种子)。2 方法2.1 样品供试液的制备取过80目筛的苦石莲皮50 g，加入正己烷4 ml和蒸馏水2 000ml，采用中国药典挥发油提取装置4提取，无水硫酸钠脱水得挥发成分，作为供试品。 取过200目筛的苦石莲皮50 g，加入正己烷4 ml和蒸馏水2000 ml，采用中国药典挥发油提取装置4提取，无水硫酸钠脱水得挥发成分，作为供试品。2.2 苦石莲挥发成分定性定量分析取样品供试液1 l进样，用GC-MS进行测定。2.2.1 气相色谱条件 色谱柱为HP-5MS 5% Phenyl Methyl Siloxane弹性石英毛细管柱(30 0.25 mm0.25 m)，柱温50，保留1min，然后以4min-1升温至280，保持2 min；汽化室温度250，载气为高纯度氦气(99.999%)，柱前压7.62psi，载气流量1.0 mlmin-1，进样量1 l，分流比401。2.2.2 质谱条件 离子源为EI源；离子源温度230 ，四极杆温度150 ；电子能量70 eV，发射电流 34.6 A，倍增器电压1637V，接口温度 280 ，溶剂延迟4min，质量范围 10550 amu。2.2.3 定性分析通过HP MSD化学工作站检索Nist98标准质谱图库和WILEY275质谱图库，同时结合有关质谱图文献解析，以确认苦石莲皮的挥发性物质的化学成分。2.2.4 定量分析并通过HP MSD 化学工作站数据处理系统，按峰面积归一化法进行计算求出各化学成分的峰面积相对百分含量。3 结果 苦石莲皮普通粉和微粉挥发性成分图谱分别见图12，各成分的峰面积相对百分含量见表1。图1 苦石莲皮普通粉挥发性物质GC-MS图谱（略）图2 苦石莲皮微粉挥发性物质GC-MS图谱（略）表1 苦石莲皮普通粉和微粉中检出挥发性成分及峰面积相对百分含量（略）4 讨论 苦石莲皮普通粉中分离出115个化学成分，鉴定出63个化学成分，检出率为54.7，其中相对百分含量大