CN108424812A - A kind of method of ultrasonic wave added isohexane extraction galic essential oil - Google Patents

A kind of method of ultrasonic wave added isohexane extraction galic essential oil Download PDF

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Publication number
CN108424812A
CN108424812A CN201810170152.4A CN201810170152A CN108424812A CN 108424812 A CN108424812 A CN 108424812A CN 201810170152 A CN201810170152 A CN 201810170152A CN 108424812 A CN108424812 A CN 108424812A
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CN
China
Prior art keywords
essential oil
isohexane
garlic
ultrasonic
galic essential
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Pending
Application number
CN201810170152.4A
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Chinese (zh)
Inventor
谢郁峰
利光辉
禹利华
吴芳
陈钰轩
罗勋方
洪卓守
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Guangdong Runhua Pharmaceutical Co ltd
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Guangdong Runhua Pharmaceutical Co ltd
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Priority to CN201810170152.4A priority Critical patent/CN108424812A/en
Publication of CN108424812A publication Critical patent/CN108424812A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction

Abstract

The invention discloses a kind of methods that ultrasonic wave added isohexane extracts galic essential oil, galic essential oil is obtained including garlic crushing, the extraction of enzymolysis, ultrasonic extraction, steam distillation, isohexane, dehydration, separation evaporation, low energy consumption for this method, oil yield is high, using isohexane as extractant, safety easily recycling, is more suitable for industrialized production.

Description

A kind of method of ultrasonic wave added isohexane extraction galic essential oil
【Technical field】
The present invention relates to a kind of extracting methods of essential oil, and in particular to a kind of ultrasonic wave added isohexane extraction galic essential oil Method.
【Background technology】
Garlic contains abundant nutriment and higher medical value.Modern study proves that garlic has anticoagulation, resists Tumour, reducing blood lipid reduce the works such as blood glucose, removing toxic substances, anti-infective, anti-oxidant, anti-aging and protection liver, protection cardiovascular system With also being played a very important role in cell-mediated immunity, humoral immunity adjustment process.
The bioactive ingredients of garlic are garlic essential oil (beneficial allicins), only account for 0.2% or so of garlic ingredient.Garlic essential oil contains More than 140 kinds of extremely precious natural materials, ingredient can totally be divided into two major classes, and one kind is volatile ingredient (also known as garlic Oil), including more than 40 kinds of sulfide compound;One kind is involatile constituent, including more than 100 kinds of esters, trace element, minerals with And various amino acid etc..The main component of galic essential oil has 6 kinds, belongs to allyl sulfide ether material, be allyl methyl thioether, Allyl sulfide, allyl methyl disulfide, diallyl disulphide, allyl methyl trisulfide ether, Diallytrisin, Diallytrisin (diallyltrisulfide) is the main component that galic essential oil has physiological activity.Also contain lemon Aldehyde (Citral), geraniol (Geraniol), linalool (Linalool), а-phellandrene (Phellan-drene), third The ingredients such as aldehyde, valeral.
Modern medicine man, biologist, medical scholar, garlic is confirmed by a large amount of scientific experimentation and clinical experiment Essential oil has six large effects:1, antibacterial, sterilize, the effect of killing the virus;2, reducing blood lipid, anti-freezing, prevention of arterial hardening, the prevention and treatment heart Cranial vascular disease;3, hypoglycemic, reduce the breaking-out of diabetes;4, liver, function of tumor inhibition are protected.By inhibiting lipid peroxy Compound reaches the damage of membrane structure liver-protective effect;5, free radical is removed, immunity of organisms is improved, it is anti-ageing Always, enhancing muscle power;6, lowering blood-fat and reducing weight;7, impotence is treated;8, improve glycometabolism.
Currently, garlic oil extracting method mainly uses steam distillation, but pass through conventional steam distillation, essential oil Isolated galic essential oil, time-consuming, oil yield is low, and Allicin Content is also low, and it is big not yet to occur the extraction of higher extracted rate at present The method of garlic essential oil.
In view of the above-mentioned problems, the present invention provides a kind of new technical solutions.
【Invention content】
The purpose of the present invention is be to have overcome the deficiencies of the prior art and provide a kind of ultrasonic wave added isohexane extraction garlic The method of essential oil can effectively improve the recovery rate of galic essential oil and the purity of galic essential oil.
In order to solve above-mentioned technical problem, the present invention uses following technical proposals:
A kind of method of ultrasonic wave added isohexane extraction galic essential oil, including have the following steps:
1. garlic clove is cleaned up, mashed garlic is worn into;
2. then, mashed garlic is added in ultrasonic extraction tank, a certain amount of water is then added in ultrasonic extraction tank, and will Water is starched with garlic and is stirred evenly in ultrasonic extraction tank, and garlic slurry is mixed into;
3. then, steam is passed through into the interlayer of ultrasonic extraction tank, when the temperature in ultrasonic extraction tank reaches 40 DEG C~45 Steam off after DEG C, garlic slurry stand enzymolysis, and the alliin in making garlic starch is digested into allicin;
4. then, ultrasonic extraction tank starts ultrasonic extraction, extracting solution is obtained after ultrasonic extraction;
5. then, steam is passed through again in the interlayer of ultrasonic extraction tank, when the temperature in ultrasonic extraction tank reaches 100 DEG C Afterwards, start steam distillation, and obtain distillate after distillation;
6. then, distillate is placed in extraction kettle, a certain amount of isohexane is added, is extracted, it is big in distillate Garlic essential oil turns to be dissolved in isohexane, obtains dissident's alkane extract;
7. then, dissident's alkane extract is carried out dehydrating with anhydrous sodium sulfate;
8. then, dissident's alkane extract after dehydration is put into separating still, after extractant evaporation, obtain remaining Liquid, as galic essential oil.
Further improvement project, in step 1, garlic clove wear into mud, after crossing 100~200 mesh, obtain mashed garlic.
Further improvement project, in step 2, the weight of the water of addition are 4~6 times of mashed garlic weight.
Further improvement project, in step 3, the supply gas pressure that steam is passed through in the interlayer of ultrasonic extraction tank are 0.1 ~0.12Mpa, standing enzymolysis time are 30~40min.
Further improvement project, in step 4, ultrasonic extraction temperature are 45 DEG C~50 DEG C, extraction time 30min, Ultrasonic power is 6000W.
Further improvement project, in steps of 5, the supply gas pressure that steam is passed through in the interlayer of ultrasonic extraction tank are 0.18 ~0.2Mpa.
Further improvement project, in step 6, the amount that isohexane is added is 2 times of distillate volume, and extraction conditions is 0.1~0.12Mpa, 30 DEG C~35 DEG C, extraction time 30min.
Further improvement project, in step 8, the oil yield of galic essential oil is 0.58%~0.65%.
The positive effect of the present invention is:The invention discloses the sides that a kind of ultrasonic wave added isohexane extracts galic essential oil Method, including garlic crushing, the extraction of enzymolysis, ultrasonic extraction, steam distillation, isohexane, dehydration, separation evaporation obtain garlic Essential oil, low energy consumption for this method, oil yield is high, and using isohexane as extractant, safety easily recycling is more suitable for industrialized production.
Below in conjunction with specific embodiment, the present invention will be further described:
【Specific implementation mode】
Embodiment one
A kind of method of ultrasonic wave added isohexane extraction galic essential oil, including have the following steps:
1. garlic clove is cleaned up, mud is worn into, is sieved with 100 mesh sieve, mashed garlic is obtained;
2. then, mashed garlic is added in ultrasonic extraction tank, water then is added in ultrasonic extraction tank, the weight of water is added It is 4 times of mashed garlic weight, and water is starched with garlic and is stirred evenly in ultrasonic extraction tank, is mixed into garlic slurry;
3. then, being passed through steam into the interlayer of ultrasonic extraction tank, the supply gas pressure of steam is 0.1Mpa, works as ultrasonic extraction Steam off after temperature in tank reaches 40 DEG C, garlic slurry stand enzymolysis, enzymolysis time 30min, the allinnase in making garlic starch Solution is at allicin;
4. then, ultrasonic extraction tank starts ultrasonic extraction, ultrasonic extraction temperature is 45 DEG C, extraction time 30min, ultrasound Power is 6000W, and extracting solution is obtained after ultrasonic extraction;
5. then, being passed through steam in the interlayer of ultrasonic extraction tank again, the supply gas pressure of steam is 0.18Mpa, works as ultrasound After temperature in extractor reaches 100 DEG C, start steam distillation, and obtain distillate after distillation;
6. then, distillate is placed in extraction kettle, isohexane is added and is extracted, the volume that isohexane is added is distillation 2 times, extraction conditions 0.1Mpa of liquid product, extraction temperature is 30 DEG C, extraction time 30min, after the extraction in distillate Galic essential oil turn be dissolved in isohexane, obtain dissident's alkane extract;
7. then, dissident's alkane extract is carried out dehydrating with anhydrous sodium sulfate;
8. then, dissident's alkane extract after dehydration is put into separating still, after extractant evaporation, obtain remaining The oil yield of liquid, as galic essential oil, galic essential oil is 0.58%.
Embodiment two
A kind of method of ultrasonic wave added isohexane extraction galic essential oil, including have the following steps:
1. garlic clove is cleaned up, mud is worn into, 150 mesh sieve is crossed, obtains mashed garlic;
2. then, mashed garlic is added in ultrasonic extraction tank, water then is added in ultrasonic extraction tank, the weight of water is added It is 5 times of mashed garlic weight, and water is starched with garlic and is stirred evenly in ultrasonic extraction tank, is mixed into garlic slurry;
3. then, being passed through steam into the interlayer of ultrasonic extraction tank, the supply gas pressure of steam is 0.11Mpa, when ultrasound carries Steam off after taking the temperature in tank to reach 43 DEG C, garlic slurry stand enzymolysis, enzymolysis time 35min, the alliin in making garlic starch Digest into allicin;
4. then, ultrasonic extraction tank starts ultrasonic extraction, ultrasonic extraction temperature is 47 DEG C, extraction time 30min, ultrasound Power is 6000W, and extracting solution is obtained after ultrasonic extraction;
5. then, being passed through steam in the interlayer of ultrasonic extraction tank again, the supply gas pressure of steam is 0.19Mpa, works as ultrasound After temperature in extractor reaches 100 DEG C, start steam distillation, and obtain distillate after distillation;
6. then, distillate is placed in extraction kettle, isohexane is added and is extracted, the volume that isohexane is added is distillation 2 times, extraction conditions 0.11Mpa of liquid product, extraction temperature is 33 DEG C, extraction time 30min, after the extraction in distillate Galic essential oil turn be dissolved in isohexane, obtain dissident's alkane extract;
7. then, dissident's alkane extract is carried out dehydrating with anhydrous sodium sulfate;
8. then, dissident's alkane extract after dehydration is put into separating still, after extractant evaporation, obtain remaining The oil yield of liquid, as galic essential oil, galic essential oil is 0.63%.
Embodiment three
A kind of method of ultrasonic wave added isohexane extraction galic essential oil, including have the following steps:
1. garlic clove is cleaned up, mud is worn into, 200 mesh sieve is crossed, obtains mashed garlic;
2. then, mashed garlic is added in ultrasonic extraction tank, water then is added in ultrasonic extraction tank, the weight of water is added It is 6 times of mashed garlic weight, and water is starched with garlic and is stirred evenly in ultrasonic extraction tank, is mixed into garlic slurry;
3. then, being passed through steam into the interlayer of ultrasonic extraction tank, the supply gas pressure of steam is 0.12Mpa, when ultrasound carries Steam off after taking the temperature in tank to reach 45 DEG C, garlic slurry stand enzymolysis, enzymolysis time 40min, the alliin in making garlic starch Digest into allicin;
4. then, ultrasonic extraction tank starts ultrasonic extraction, ultrasonic extraction temperature is 50 DEG C, extraction time 30min, ultrasound Power is 6000W, and extracting solution is obtained after ultrasonic extraction;
5. then, being passed through steam in the interlayer of ultrasonic extraction tank again, the supply gas pressure of steam is 0.2Mpa, when ultrasound carries After taking the temperature in tank to reach 100 DEG C, start steam distillation, and obtain distillate after distillation;
6. then, distillate is placed in extraction kettle, isohexane is added and is extracted, the volume that isohexane is added is distillation 2 times, extraction conditions 0.12Mpa of liquid product, extraction temperature is 35 DEG C, extraction time 30min, after the extraction in distillate Galic essential oil turn be dissolved in isohexane, obtain dissident's alkane extract;
7. then, dissident's alkane extract is carried out dehydrating with anhydrous sodium sulfate;
8. then, dissident's alkane extract after dehydration is put into separating still, after extractant evaporation, obtain remaining The oil yield of liquid, as galic essential oil, galic essential oil is 0.65%.
Garlic clove in the present invention in embodiment one, embodiment two and embodiment three is all made of Shandong garlic, and isohexane uses The isohexane that Herpu Chemical Co., Ltd., Guangzhou provides.
The invention discloses a kind of methods (extraction process) that ultrasonic wave added isohexane extracts galic essential oil, including garlic powder Broken, enzymolysis, ultrasonic extraction, steam distillation, isohexane extraction, dehydration, separation evaporation obtain galic essential oil, this method energy Consume that low, oil yield is high, using isohexane as extractant, safety easily recycling is more suitable for industrialized production.
It is aobvious for those skilled in the art by the disclosure although the present invention is described in detail with reference to above example And be clear to, and in the case where not departing from the principle of the present invention and scope that the claim limits, it can be right The present invention makes a variety of changes or changes.Therefore, the detailed description of the embodiment of the present disclosure is only used for explaining, rather than for limiting The present invention, but it is defined by the subject-matter of the claims the range of protection.It is all identical with application scheme, approximate or based on this Technology deduction, replacement, improvement for making etc., are regarded as the protection domain of this patent.

Claims (8)

1. a kind of method of ultrasonic wave added isohexane extraction galic essential oil, which is characterized in that including having the following steps:
1. garlic clove is cleaned up, mashed garlic is worn into;
2. then, mashed garlic is added in ultrasonic extraction tank, be then added a certain amount of water in ultrasonic extraction tank, and by water with Garlic slurry stirs evenly in ultrasonic extraction tank, is mixed into garlic slurry;
3. then, steam is passed through into the interlayer of ultrasonic extraction tank, after the temperature in ultrasonic extraction tank reaches 40 DEG C~45 DEG C Steam off, garlic slurry stand enzymolysis, and the alliin in making garlic starch is digested into allicin;
4. then, ultrasonic extraction tank starts ultrasonic extraction, extracting solution is obtained after ultrasonic extraction;
5. then, being passed through steam again in the interlayer of ultrasonic extraction tank, after the temperature in ultrasonic extraction tank reaches 100 DEG C, open Beginning steam distillation, and distillate is obtained after distillation;
6. then, distillate is placed in extraction kettle, a certain amount of isohexane is added, is extracted, the garlic essence in distillate Oil turns to be dissolved in isohexane, obtains dissident's alkane extract;
7. then, dissident's alkane extract is carried out dehydrating with anhydrous sodium sulfate;
8. then, dissident's alkane extract after dehydration is put into separating still, after extractant evaporation, extraction raffinate is obtained, i.e., For galic essential oil.
2. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 1, which is characterized in that In step 1, garlic clove wears into mud, after crossing 100~200 mesh sieve, obtains mashed garlic.
3. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 2, which is characterized in that In step 2, the weight of the water of addition is 4~6 times of mashed garlic weight.
4. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 3, which is characterized in that In step 3, be passed through in the interlayer of ultrasonic extraction tank steam supply gas pressure be 0.1~0.12Mpa, stand enzymolysis time be 30~ 40min。
5. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 4, which is characterized in that In step 4, ultrasonic extraction temperature is 45 DEG C~50 DEG C, extraction time 30min, ultrasonic power 6000W.
6. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 5, which is characterized in that In step 5, the supply gas pressure that steam is passed through in the interlayer of ultrasonic extraction tank is 0.18~0.2Mpa.
7. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 6, which is characterized in that In step 6, the amount that isohexane is added is 2 times of distillate volume, and extraction conditions is 0.1~0.12Mpa, 30 DEG C~35 DEG C, is extracted It is 30min to take the time.
8. the method for extracting galic essential oil according to a kind of ultrasonic wave added isohexane described in claim 7, which is characterized in that In step 8, the oil yield of galic essential oil is 0.58%~0.65%.
CN201810170152.4A 2018-03-01 2018-03-01 A kind of method of ultrasonic wave added isohexane extraction galic essential oil Pending CN108424812A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109601559A (en) * 2019-01-07 2019-04-12 贵州省烟草公司遵义市公司 It is a kind of prevent and treat phytophthora mother chrysanthemum essential oil and its application
CN109609272A (en) * 2018-11-23 2019-04-12 盐城工学院 A kind of extracting method for the galic essential oil reducing cholesterol micella solubility

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849468A (en) * 2014-03-12 2014-06-11 青海清华博众生物技术有限公司 Garlic essential oil extraction method
CN106367208A (en) * 2016-11-25 2017-02-01 徐州黎明食品有限公司 Separation and purification method of garlic essential oil
CN107603741A (en) * 2017-09-28 2018-01-19 江永百润福天然植物科技发展有限公司 A kind of preparation method and galic essential oil that galic essential oil is extracted from garlic

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849468A (en) * 2014-03-12 2014-06-11 青海清华博众生物技术有限公司 Garlic essential oil extraction method
CN106367208A (en) * 2016-11-25 2017-02-01 徐州黎明食品有限公司 Separation and purification method of garlic essential oil
CN107603741A (en) * 2017-09-28 2018-01-19 江永百润福天然植物科技发展有限公司 A kind of preparation method and galic essential oil that galic essential oil is extracted from garlic

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109609272A (en) * 2018-11-23 2019-04-12 盐城工学院 A kind of extracting method for the galic essential oil reducing cholesterol micella solubility
CN109601559A (en) * 2019-01-07 2019-04-12 贵州省烟草公司遵义市公司 It is a kind of prevent and treat phytophthora mother chrysanthemum essential oil and its application
CN109601559B (en) * 2019-01-07 2021-01-15 贵州省烟草公司遵义市公司 Wild chrysanthemum essential oil for preventing and treating phytophthora and application thereof

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