CN105695096A - 细梗香草提取液及其制备方法 - Google Patents
细梗香草提取液及其制备方法 Download PDFInfo
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- herba lysimachiae
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
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- 238000000605 extraction Methods 0.000 title description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
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- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
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- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 1
- CDOSHBSSFJOMGT-UHFFFAOYSA-N beta-linalool Natural products CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 1
- 201000008275 breast carcinoma Diseases 0.000 description 1
- WFCLHMCZUVCIHV-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O.CC(O)C(C)O WFCLHMCZUVCIHV-UHFFFAOYSA-N 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 229930189274 capilliposide Natural products 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- RFFOTVCVTJUTAD-UHFFFAOYSA-N cineole Natural products C1CC2(C)CCC1(C(C)C)O2 RFFOTVCVTJUTAD-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 description 1
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
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- 150000002596 lactones Chemical class 0.000 description 1
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- 238000004949 mass spectrometry Methods 0.000 description 1
- UTGAUYRMSGONEZ-UHFFFAOYSA-N octanal Chemical compound CCCCCCCC=O.CCCCCCCC=O UTGAUYRMSGONEZ-UHFFFAOYSA-N 0.000 description 1
- RUVINXPYWBROJD-UHFFFAOYSA-N para-methoxyphenyl Natural products COC1=CC=C(C=CC)C=C1 RUVINXPYWBROJD-UHFFFAOYSA-N 0.000 description 1
- KVYJZMJPHSXEDZ-UHFFFAOYSA-N pentan-1-ol Chemical compound CCCCCO.CCCCCO KVYJZMJPHSXEDZ-UHFFFAOYSA-N 0.000 description 1
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- UNYNVICDCJHOPO-UHFFFAOYSA-N sotolone Chemical compound CC1OC(=O)C(O)=C1C UNYNVICDCJHOPO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
本发明公开了细梗香草提取液及其制备方法，旨在提供一种天然的细梗香草提取液及其制备方法，生产成本低，所得细梗香草提取液是一种香精原料、食品添加剂、日化添加剂和药品原料。作为香精原料，其香气清雅，广泛用于化妆品和日用化工；作为食品药品原料，不仅具有增香剂作用，还具有抗癌和治疗心血管病的作用。其技术方案，依次包括下述步骤：（1)制备：用超临界二氧化碳法萃取细梗香草精油；(2)检验：气相色谱质谱联用仪分析天然香草细梗香草精油成分；（3）成品。
Description
技术领域
本发明公开了细梗香草提取液及其制备方法，具体地说，是一种天然的细梗香草提取液及其制备方法；属于香精香料配方和技术领域。
背景技术
香产品历来为高级消费品，随着物质生活水品的提高其越来越重要。对比化学配置的香料，天然香精更珍贵高雅。
细梗香草又名细梗香、满山香、排草、香草等，报春花科、珍珠菜族，其茎叶含芳香油。细梗香草精油气质联用色谱法分析，获得28种化合物，其中包括大茴香脑、咖啡碱等大量芳香物质和细梗香草皂苷等药用成分。文献显示，细梗香草的提取液对卵巢癌、前列腺癌、胃癌、肺癌、乳腺癌等的癌细胞等有显著的抑制作用。长期以来，细梗香草就是作为一种药草运用于民间，也用作茶叶的提香剂，但并未作为香精原料提取和使用。能够在食品、药品、日用化工和护肤化妆品中广泛应用且具有抗癌作用的细梗香草提取液，具有广阔的发展前景。
发明内容
针对上述不足，本发明的目的在于，以天然的细梗香草为原料获得提取液。以超临界二氧化碳法萃取细梗香草菁华，去杂过滤提纯，制备方法简单，生产成本低，所得细梗香草提取液香味高雅，应用十分广泛。
为此，本发明提供的技术方案是这样的：细梗香草提取液的制备方法，包括下述步骤：（1)用超临界二氧化碳法萃取细梗香草提取液；(2)气相色谱质谱联用仪分析天然香草细梗香草提取液成分。（3）成品封装。
所述的超临界二氧化碳法萃取细梗香草精油的过程是：将细梗香草粉碎成过60目筛的粗粉；将细梗香草粉放入萃取釜，打开二氧化碳使其与细梗香草粉充分接触并保持12小时-20小时，再进行超临界萃取；在超临界萃取过程中将夹带剂由副泵打入萃取釜中。所述的超临界萃取中，二氧化碳流体的萃取温度为40-55℃，压力为12-35MPa；分离釜的分离温度为35-50℃；压力为8-10MPa；主泵流量为60-120kg/hr；副泵流量为30-90kg/hr；萃取时间为60-120min。所述的夹带剂是无水乙醇。夹带剂的量为细梗香草粉重量的0.5-2倍。所述的分离釜是一个或多个。
具体实施方式
下面结合具体实施方式，对本发明的权利要求做进一步的详细说明，但不构成对本发明的任何限制，任何人在本发明权利要求范围内所做的有限次的修改，仍在本发明的权利要求保护范围之内。
实施例1：细梗香草粉碎60目过筛；将细梗香草粉放入萃取釜，打开二氧化碳使其与细梗香草粉充分接触并保持12小时-20小时，再进行超临界萃取；将相当于细梗香草粉0.8倍的无水乙醇作为夹带剂由副泵打入萃取釜中。超临界萃取中，二氧化碳流体的萃取温度为40-55℃，压力为12-35MPa；分离釜的分离温度为35-50℃；压力为8-10MPa；主泵流量为60-120kg/hr；副泵流量为30-90kg/hr；萃取时间为60-120min。萃取完毕，回收萃取液封装待检。
实施例2：气相色谱质谱联用仪分析天然香草细梗香草提取液成分：内标物癸醇，浓度为0.00274/0.2；仪器型号和进样条件：Agilent6890-5973；色谱条件：进样口温度：250度；色谱柱型号：HP-5,60m*0.25mm*0.25um；进样条件：50度，10度每分钟到100度，保持5分钟，3度每分钟到140度,保持10分钟，2度每分钟到230度，保持10min；载气：He，流速：1ml/min,进样量：0.2ul，不分流；质谱条件：离子源：230度，四级杆温度：150度。
分析结果如下表：
| 序号 | 出峰时间(min) | mg/g | 物质 |
| 1 | 4.923 | 48.657 | 乙醇 Ethanol（夹带剂） |
| 2 | 5.217 | 0.219 | 丙醇 1-Propanol |
| 3 | 5.39 | 0.319 | 乙酸 Acetic acid |
| 4 | 6.383 | 0.080 | 3-羟基-2-丁酮，2-Butanone, 3-hydr |
| 5 | 6.709 | 0.040 | 2－甲基－2－丁烯醛2-Butenal, 2-met |
| 6 | 6.959 | 0.027 | 戊醇 1-Pentanol |
| 7 | 7.215 | 0.040 | 2,3-丁二醇 2,3-Butanediol |
| 8 | 7.868 | 0.040 | 3-甲基丁酸 Butanoic acid, 3-methyl |
| 9 | 8.035 | 0.027 | 2-甲基丁酸 Butanoic acid, 2-methyl- |
| 10 | 9.623 | 0.027 | 2-甲基丁烯酸 2-Butenoic acid, 2-m |
| 11 | 10.014 | 0.020 | 丁内酯 Butyrolactone |
| 12 | 11.365 | 0.020 | 己酸 Hexanoic acid |
| 13 | 11.922 | 0.033 | 顺-3-己烯酸 (3Z)-3-HEXENOIC ACID |
| 14 | 14.138 | 0.007 | dl-柠檬烯 dl-Limonene |
| 15 | 14.227 | 0.007 | 苯甲醇 Benzyl Alcohol |
| 16 | 14.355 | 0.007 | 桉叶素 Eucalyptol |
| 17 | 15.277 | 0.007 | 2-乙酰基吡咯 Ethanone, 1-(1H-pyrrol-2-yl)- |
| 18 | 15.476 | 0.033 | 1-辛醇 1-Octanol |
| 19 | 16.782 | 0.080 | 葫芦巴内酯(3-羟基-4,5-二甲基-2(5H)-呋喃酮) |
| 20 | 18.377 | 0.013 | 辛醛 Octanal |
| 21 | 18.959 | 0.013 | 2,3-二氢-3,5-二羟基-6-甲基-4H-吡喃-4-酮 2,3-Dihydro-3,5-dihydroxy-6- |
| 22 | 19.35 | 0.007 | 苯甲酸 Benzoic acid |
| 23 | 21.572 | 0.013 | 二氢大茴香脑 Benzene, 1-methoxy-4- |
| 24 | 23.128 | 0.053 | 3-氨基-4,5-二甲基-2(5H)-呋喃酮 3-Amino-4,5-dimethyl-2(5H)-furanon |
| 25 | 24.351 | 0.013 | 大茴香醛 Anisic Aldehyde |
| 26 | 24.979 | 13.700 | 癸醇 1-Decanol (内标物) |
| 27 | 25.895 | 0.213 | 大茴香脑 Anethole |
| 28 | 28.879 | 0.053 | 8-羟基芳樟醇 |
| 29 | 62.958 | 0.525 | 咖啡碱 Caffeine |
| 30 | 77.661 | 0.106 | 9,12,15-十八碳三烯-1-醇 |
Claims (4)
1.一种细梗香草提取液，其特征在于，其由天然的细梗香草提炼而成。
2.一种细梗香草提取液的制备方法，其特征在于，包括下述步骤：（1)制备：用超临界二氧化碳法萃取细梗香草精油；(2)检验：气相色谱质谱联用仪分析天然香草细梗香草精油成分；（3）成品。
3.一种细梗香草提取液的应用领域，其特征在于，细梗香草提取液是一种香精原料、食品添加剂、日化添加剂和药品原料。
4.作为香精原料，其香气清雅，广泛用于化妆品和日用化工；作为食品药品原料，不仅具有增香剂作用，还具有抗癌和治疗心血管病的作用。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108982743A (zh) * | 2018-08-17 | 2018-12-11 | 福建中烟工业有限责任公司 | 检测烟草制品和/或烟用香精香料中葫芦巴内酯的方法 |
| CN114264763A (zh) * | 2021-12-22 | 2022-04-01 | 金绿源(中国)生物科技有限公司 | 一种细梗香草的取样方法 |
Citations (2)
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| CN102180938A (zh) * | 2011-03-30 | 2011-09-14 | 浙江大学 | 细梗香草皂苷的制备方法 |
| CN102228488A (zh) * | 2011-06-07 | 2011-11-02 | 南京泽朗农业发展有限公司 | 一种细梗香草总皂苷的制备方法 |
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| CN102180938A (zh) * | 2011-03-30 | 2011-09-14 | 浙江大学 | 细梗香草皂苷的制备方法 |
| CN102228488A (zh) * | 2011-06-07 | 2011-11-02 | 南京泽朗农业发展有限公司 | 一种细梗香草总皂苷的制备方法 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982743A (zh) * | 2018-08-17 | 2018-12-11 | 福建中烟工业有限责任公司 | 检测烟草制品和/或烟用香精香料中葫芦巴内酯的方法 |
| CN114264763A (zh) * | 2021-12-22 | 2022-04-01 | 金绿源(中国)生物科技有限公司 | 一种细梗香草的取样方法 |
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