CN103389354A - 香荚兰豆药材中挥发性成分的分析方法 - Google Patents
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Abstract
本发明公开了一种香荚兰豆药材中挥发性成分的分析方法。本发明以香荚兰豆药材为原料,首先采用顶空固相微萃取提取香荚兰豆挥发性成分,再采用气相色谱-质谱联用法对其挥发性成分进行分析,经化学工作站数据处理及用面积归一化法从总离子流图中计算各组分百分含量,按各峰的质谱图经NIST谱库检索,并按各峰的质谱裂片图与文献资料核对,确定各个组分。本发明首次采用顶空固相微萃取结合气相色谱-质谱联用法对香荚兰豆药材中挥发性成分进行提取与分析,弥补了以往提取方法对挥发性成分提取不完全的缺点,为该药材挥发性成分的分离分析提供更为全面的检测方法。
Description
技术领域
本发明涉及药材中化学成分的分析方法,具体地指一种香荚兰豆药材中挥发性成分的分析方法。
背景技术
香荚兰豆为兰科香荚兰属植物香荚兰Vanilla planifoli Andrews的成熟果实,原产于非洲岛国马达加斯加,我国云南西双版纳等地已引进栽培。香荚兰豆具有息风止痉、镇静抗惊等功效。现代研究表明它还具有镇静、抗惊厥、抗氧化及抑菌等药理活性,其主要化学成分为醛类、酚类、萜类、酯类、挥发油、糖类及有机酸等。香荚兰豆是一种名贵的天然食品香料,因其丰满、浓郁的香气而被广泛地应用于医药、食品等领域。
目前,国内对香荚兰豆挥发性成分的提取方法仅见超临界二氧化碳萃取(SFE-CO2)和同时蒸馏萃取(SDE)法,分析方法多为气相色谱-质谱联用法(GC-MS)。SFE-CO2法对不同物质的溶解能力差别较大,与物质的极性、沸点和相对分子质量有密切的关系,对于亲脂性成分萃取较完全,对于中等极性成分(如皂苷、黄酮苷)或极性更大的成分无法萃取。而SDE法的蒸馏温度过高,样品可能发生水解、氧化、酯化或热分解,同时高沸点的组分也难以随水蒸气一起蒸出来。所以二者均不能全面反映样品中挥发性成分的真实组成。
另外,因香荚兰的品种、产地和加工方法的差异导致挥发性成分在组成和含量上的差异,难以对香荚兰豆药材质量进行全面客观的评价。
发明内容
本发明的目的就是要克服现有技术所存在的不足,提供一种香荚兰豆药材中挥发性成分的分析方法。
为实现上述目的,本发明所提供的香荚兰豆药材中挥发性成分的分析方法,它包括以下步骤:
(a)顶空固相微萃取提取挥发性成分:
取香荚兰豆原药材2.0g,剪碎,置于固相微萃取仪顶空瓶中,用带有65μm聚二甲基硅氧烷-二乙烯基苯萃取纤维头的手动进样器插入瓶内,90℃平衡30min,再顶空萃取20min,取出,立即插入气相色谱仪进样口,进样口温度为250℃,解吸3min,进样模式为不分流进样;
(b)气相色谱-质谱联用分析条件:
色谱条件:色谱柱:HP-5MS石英毛细管柱,其尺寸为50m×0.2mm×0.33μm;程序升温:初始温度30℃,以2℃/min升温至80℃,保留2min,再以10℃/min升温至250℃,保留5min;进样口温度:250℃;载气:高纯氦气;载气流速:1.0mL/min;
质谱条件:离子源:EI源;离子源温度:230℃;四级杆温度:150℃;电子能量:70eV;倍增管电压:1.2kV;接口温度:280℃;质量范围:35~550m/z;
(c)挥发性成分的定性及定量分析:
定性分析通过化学工作站检索NIST标准质谱图库,同时结合有关质谱图文献解析,确认香荚兰豆挥发性成分;定量分析通过化学工作站数据处理系统,按峰面积归一化法进行计算,求出各组分的相对百分含量。
顶空固相微萃取法(英文简称为HS-SPME)具有萃取速度快、操作简便、富集效率高的特点。
本发明采用顶空固相微萃取结合气相色谱-质谱联用法(即HS-SPME-GC-MS)对香荚兰豆药材中挥发性成分进行了提取与分析,共分离出32个峰,确定了其中28个组分,香荚兰豆挥发性成分中,主要为醛类,还含有酚类、醇类、酸类、酯类、酮类、烯烃类等,其中含量最高的为香兰素(48.28%),其次为愈创木酚(15.54%),这2种化合物的含量占挥发性成分总量的63.82%。
本发明首次采用顶空固相微萃取结合气相色谱-质谱联用法(HS-SPME-GC-MS)对香荚兰豆药材中挥发性成分进行提取与分析,弥补了以往提取方法对挥发性成分提取不完全的缺点,为该药材挥发性成分的分离分析提供更为全面的检测方法。
附图说明
图1为香荚兰豆中挥发性成分GC-MS总离子流图。
具体实施方式
以下结合附图和具体实施例对本发明作进一步的详细描述。
实施例1
(a)顶空固相微萃取(HS-SPME)提取挥发性成分:
取香荚兰豆原药材2.0g,剪碎,置于固相微萃取仪顶空瓶中,用带有65μm聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)萃取纤维头的手动进样器插入瓶内,90℃平衡30min,再顶空萃取20min,取出,立即插入气相色谱仪进样口(温度250℃);解吸3min;进样模式为不分流进样。
(b)气相色谱-质谱联用(GC-MS)分析条件:
色谱条件:色谱柱:HP-5MS石英毛细管柱,其尺寸为50m×0.2mm×0.33μm;程序升温:初始温度30℃,以2℃/min升温至80℃,保留2min,再以10℃/min升温至250℃,保留5min;进样口温度:250℃;载气:高纯氦气;载气流速:1.0mL/min;
质谱条件:离子源:EI源;离子源温度:230℃;四级杆温度:150℃;电子能量:70eV;倍增管电压:1.2kV;接口温度:280℃;质量范围:35~550m/z;
(c)挥发性成分定性及定量分析:
定性分析通过HP-MSD化学工作站检索NIST标准质谱图库,同时结合有关质谱图文献解析,确认香荚兰豆挥发性成分。定性分析所得的香荚兰豆中挥发性成分GC-MS总离子流图如图1所示。
定量分析通过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,求出各组分的相对百分含量。香荚兰豆中挥发性成分的定量分析结果如表1所示。
表1香荚兰豆中挥发性成分的定量分析结果
本发明共分离出32个峰,确定了其中28个组分,香荚兰豆中挥发性成分,主要为醛类,还含有酚类、醇类、酸类、酯类、酮类、烯烃类等,其中含量最高的为香兰素(48.28%),其次为愈创木酚(15.54%),这2种化合物的含量占挥发性成分总量的63.82%。
Claims (1)
1.一种香荚兰豆药材中挥发性成分的分析方法,其特征在于,它包括以下步骤:
(a) 顶空固相微萃取提取挥发性成分:
取香荚兰豆原药材2.0g,剪碎,置于固相微萃取仪顶空瓶中,用带有65μm聚二甲基硅氧烷-二乙烯基苯萃取纤维头的手动进样器插入瓶内,90℃平衡30min,再顶空萃取20min,取出,立即插入气相色谱仪进样口,进样口温度为250℃,解吸3min,进样模式为不分流进样;
(b) 气相色谱-质谱联用分析条件:
色谱条件:色谱柱:HP-5MS石英毛细管柱,其尺寸为50m×0.2mm×0.33μm;程序升温:初始温度30℃,以2℃/min升温至80℃,保留2min,再以10℃/min升温至250℃,保留5min;进样口温度:250℃;载气:高纯氦气;载气流速:1.0mL/min;
质谱条件:离子源:EI源;离子源温度:230℃;四级杆温度:150℃;电子能量:70eV;倍增管电压:1.2kV;接口温度:280℃;质量范围:35~550m/z;
(c) 挥发性成分的定性及定量分析:
定性分析通过化学工作站检索NIST标准质谱图库,同时结合有关质谱图文献解析,确认香荚兰豆挥发性成分;定量分析通过化学工作站数据处理系统,按峰面积归一化法进行计算,求出各组分的相对百分含量。
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CN107974351A (zh) * | 2017-12-29 | 2018-05-01 | 丽华(广州)香精香料股份有限公司 | 一种超声波辅助超临界二氧化碳萃取香荚兰豆精油的方法 |
CN114324664A (zh) * | 2021-12-30 | 2022-04-12 | 广州酒家集团利口福食品有限公司 | 一种检测莲蓉馅料中挥发性成分的方法 |
CN114324664B (zh) * | 2021-12-30 | 2024-05-03 | 广州酒家集团利口福食品有限公司 | 一种检测莲蓉馅料中挥发性成分的方法 |
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