CN103336086A - 咖啡豆药材中挥发油化学成分的分析方法 - Google Patents
咖啡豆药材中挥发油化学成分的分析方法 Download PDFInfo
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
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- BRBUBVKGJRPRRD-UHFFFAOYSA-N 4,6-dimethylpyridin-2-amine Chemical class CC1=CC(C)=NC(N)=C1 BRBUBVKGJRPRRD-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种咖啡豆药材中挥发油化学成分的分析方法。本发明以咖啡豆药材为原料,首次采用水蒸气蒸馏的方法提取咖啡豆中的挥发油,再采用气相色谱-质谱联用法对其挥发油化学成分进行测定分析,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相对百分含量,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。本发明为咖啡豆药材的质量控制提供理论基础,为咖啡豆的综合利用提供科学依据。
Description
技术领域
本发明涉及药材中化学成分的分析方法,具体地指一种咖啡豆药材中挥发油化学成分的分析方法。
背景技术
咖啡豆为茜草科咖啡属植物小果咖啡Coffea arabica L、中果咖啡C.canephora Pierre ex Froehn及大果咖啡C.liberica Bull.ExHien的种子,产自巴西、哥伦比亚等地,在中国主要产于云南、海南、广东等地,味微苦、涩,具有醒神、利尿、健胃等功效,主治精神怠倦,食欲不振,现代研究还表明其具有兴奋中枢、降血压、抗氧化、抗肿瘤等作用。
咖啡豆中主要的化学成分为生物碱类、多酚类、油脂类以及碳水化合物。咖啡豆因其味道甘醇,有独特香味,是世界上最受欢迎的三大饮品之一,同时由于咖啡豆中含有大量的油脂类成分和挥发性香气成分,已被广泛应用于烟草行业及香精香料行业中。
水蒸气蒸馏法(SD)是提取植物中挥发油的经典方法。国内尚未见采用水蒸气蒸馏(SD)结合气相色谱-质谱联用(GC-MS)法对咖啡豆药材挥发油化学成分进行分析的报道。
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,提供一种咖啡豆药材中挥发油化学成分的分析方法。
为实现上述目的,本发明所提供的咖啡豆药材中挥发油化学成分的分析方法,它包括以下步骤:
(a)供试品溶液的制备:
取咖啡豆药材,粉碎过20目筛,取粗粉加10倍重量的水,浸泡8h,常压水蒸气蒸馏连续提取挥发油10h,加乙醚萃取,取上层溶液,即得供试品溶液;
(b)测定方法及条件:
取供试品溶液1μL,再采用气相色谱-质谱联用法对其挥发油化学成分进行测定分析,
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:50℃保留,以3℃/min升温至70℃,再以5℃/min升温至90℃,最后以8℃/min升温至220℃,保留2min;分流比10:1;溶剂延时:3min;
质谱条件:离子源:EI源;离子源温度:230℃;四极杆温度:150℃;倍增管电压:1.2kV;进样口温度:230℃;质量范围:35~550m/z。
(c)挥发油化学成分定性及定量分析:
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,确认咖啡豆挥发油中各组分;定量分析通过化学工作站数据处理系统,按峰面积归一化法从总离子流图中进行计算求出各组分相对百分含量。
本发明的有益效果在于:本发明采用水蒸气蒸馏(SD)结合气相色谱-质谱联用(GC-MS)法对咖啡豆药材中挥发油化学成分进行提取与分析。本发明在咖啡豆挥发油中共分离出29个峰,确定了其中27个组分,其中含量较高的为2-甲氧基-3-烯丙基苯酚(18.75%)、2,6-二甲基吡嗪(13.55%)、棕榈酸(12.81%)、2-氨基-4,6-二甲基吡啶(11.58%)、5-甲基糠醛(7.52%)。本发明为该药材的质量控制提供理论基础,为咖啡豆的综合利用提供科学依据。
附图说明
图1为咖啡豆挥发油化学成分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)供试品溶液的制备:
取咖啡豆药材,粉碎过20目筛,取适量粗粉加10倍重量的水,浸泡8h,常压水蒸气蒸馏连续提取挥发油10h,得油状液体0.061g,加1mL乙醚萃取,取上层溶液,即得供试品溶液;
(b)测定方法及条件:
取供试品溶液1μL,再采用GC-MS气对其挥发油化学成分进行测定分析,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:50℃保留,以3℃/min升温至70℃,再以5℃/min升温至90℃,最后以8℃/min升温至220℃,保留2min;分流比10:1;溶剂延时:3min;
质谱条件:离子源:EI源;离子源温度:230℃;四极杆温度:150℃;倍增管电压:1.2kV;进样口温度:230℃;质量范围:35~550m/z。
(c)挥发油化学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,确认咖啡豆挥发油的化学成分。定性分析所得的咖啡豆挥发油化学成分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,按峰面积归一化法从总离子流图中进行计算求出化学成分的峰面积相对百分含量。咖啡豆挥发油化学成分的定量分析结果如表1所示。
表1 咖啡豆挥发油化学成分的定量分析结果
本发明在咖啡豆挥发油中共分离出29个峰,确定了其中27个组分,其中含量较高的为2-甲氧基-3-烯丙基苯酚(18.75%)、2,6-二甲基吡嗪(13.55%)、棕榈酸(12.81%)、2-氨基-4,6-二甲基吡啶(11.58%)、5-甲基糠醛(7.52%)。本发明为该药材的质量控制提供理论基础,为咖啡豆的综合利用提供科学依据。
Claims (1)
1.一种咖啡豆药材中挥发油化学成分的分析方法,其特征在于,它包括以下步骤:
(a) 供试品溶液的制备:
取咖啡豆药材,粉碎过20目筛,取粗粉加10倍重量的水,浸泡8h,常压水蒸气蒸馏连续提取挥发油10h,加乙醚萃取,取上层溶液,即得供试品溶液;
(b) 测定方法及条件:
取供试品溶液1μL,再采用气相色谱-质谱联用法对其挥发油化学成分进行测定分析,
色谱条件:色谱柱:HP-5MS石英毛细管柱,尺寸50m×0.2mm×0.33μm;程序升温:50℃保留,以3℃/min升温至70℃,再以5℃/min升温至90℃,最后以8℃/min升温至220℃,保留2min;分流比10:1;溶剂延时:3min;
质谱条件:离子源:EI源;离子源温度:230℃;四极杆温度:150℃;倍增管电压:1.2kV;进样口温度:230℃;质量范围:35~550m/z。
(c) 挥发油化学成分定性及定量分析:
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,确认咖啡豆挥发油中各组分;定量分析通过化学工作站数据处理系统,按峰面积归一化法从总离子流图中进行计算求出各组分相对百分含量。
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WO2015192834A3 (de) * | 2014-06-18 | 2016-04-14 | Klaus Hagen | Verfahren zur herstellung eines zur verdampfung vorgesehenen verbrauchsstoffs |
CN107179368A (zh) * | 2017-06-15 | 2017-09-19 | 云南中烟工业有限责任公司 | 一种提升烟气感官得分的香气成分的检测及判定方法 |
CN112858508A (zh) * | 2021-01-13 | 2021-05-28 | 浙江省疾病预防控制中心 | 一种咖啡制品中糠醛类化合物的测定方法 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015192834A3 (de) * | 2014-06-18 | 2016-04-14 | Klaus Hagen | Verfahren zur herstellung eines zur verdampfung vorgesehenen verbrauchsstoffs |
CN107179368A (zh) * | 2017-06-15 | 2017-09-19 | 云南中烟工业有限责任公司 | 一种提升烟气感官得分的香气成分的检测及判定方法 |
CN107179368B (zh) * | 2017-06-15 | 2019-01-08 | 云南中烟工业有限责任公司 | 一种提升烟气感官得分的香气成分的检测及判定方法 |
CN112858508A (zh) * | 2021-01-13 | 2021-05-28 | 浙江省疾病预防控制中心 | 一种咖啡制品中糠醛类化合物的测定方法 |
CN112858508B (zh) * | 2021-01-13 | 2022-10-18 | 浙江省疾病预防控制中心 | 一种咖啡制品中糠醛类化合物的测定方法 |
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