WO2020211562A1 - 一种从大麻中提取挥发油的方法及挥发油的应用 - Google Patents

一种从大麻中提取挥发油的方法及挥发油的应用 Download PDF

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WO2020211562A1
WO2020211562A1 PCT/CN2020/078031 CN2020078031W WO2020211562A1 WO 2020211562 A1 WO2020211562 A1 WO 2020211562A1 CN 2020078031 W CN2020078031 W CN 2020078031W WO 2020211562 A1 WO2020211562 A1 WO 2020211562A1
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volatile oil
hemp
cannabis
heating
temperature
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PCT/CN2020/078031
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French (fr)
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于朝晖
常坦然
高伟博
柳旭
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云南汉盟制药有限公司
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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26—Use of organic solvents for extraction
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303—Plant extracts other than tobacco
    • 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)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A—HUMAN NECESSITIES
    • 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
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]

Definitions

  • the invention relates to the fields of tobacco and food, and in particular to a method for extracting volatile oil from hemp.
  • the chemical composition of industrial hemp is very complex, mainly including lipids, flavonoids, terpenes, hydrocarbons, non-cyclic macrophenols, alkaloids, silver citrate and cyclic cannabinol.
  • Humans have a history of smoking marijuana for more than a thousand years.
  • the special aroma of marijuana mainly comes from terpene components.
  • the terpene components in marijuana can be used as cigarette flavors and food flavors, which has extremely high economic value; but its It is highly volatile.
  • active substances such as cannabinol substances
  • terpene components are often directly discharged, resulting in a great waste of resources.
  • the present invention provides a method for extracting volatile oil from hemp.
  • the method of the present invention can solve the technical drawbacks of the prior art that the volatile oil components of hemp are not used but are discharged together with the exhaust gas; and
  • the method of the present invention requires less organic solvent and low residual organic solvent.
  • the obtained volatile oil has a unique aroma of cannabis.
  • the present invention provides the following technical solutions:
  • a method for extracting volatile oil from hemp includes the following steps:
  • step 2) The dried hemp flowers and leaves after step 1) are dried and dehydrated into powder, and the hemp seeds are removed, for example, the wrapped hemp seeds are removed by winnowing;
  • step 2) Place the hemp flower and leaf material processed in step 2) in a heating and drying device at a heating temperature of 100-120°C (for example, 100°C, 105°C, 110°C, 115°C, 120°C, etc.); the heating and drying
  • the air outlet of the device is connected to a condensing device, which condenses the gas discharged from the air outlet and obtains condensate containing volatile oil;
  • the extractant is preferably selected from ethyl acetate, n-heptane, n-butanol, n-hexane, dichloromethane, One or a combination of two or more in petroleum ether, using a preferred extractant, has a high yield of volatile oil, and can better dissolve terpenes;
  • step 5) Wash the supernatant obtained in step 4) with water and remove the water layer, and distill the obtained organic layer to obtain hemp volatile oil.
  • step 1) the water content of hemp flowers and leaves is controlled at 20%-30% by weight, which facilitates the removal of volatile oil in step 3) and improves the extraction rate of volatile oil; and if the moisture content is too low, it will make the volatile oil It is not easy to be taken out during the subsequent heating and drying; and if the moisture content is too high, the energy consumption will increase due to the excessive humidity of the material.
  • step 3 heating and drying are carried out at 100-120°C.
  • the cannabidiol acid components can undergo decarboxylation reaction, which is beneficial to the subsequent cannabidiol substances
  • the subsequent extraction process can increase the yield of cannabidiol components.
  • the main components of the cannabis volatile oil obtained by the method of the present invention are terpenes, and the characteristic components include, for example, p-cymene, ⁇ -bisabolol, ocimene, ⁇ -terpinene, ⁇ -caryophyllene, guaiacol, Geraniol, ⁇ -pinene, ⁇ -ocimene, terpinene, ⁇ -pinene, trans-neryl alcohol, 4-methoxybenzyl alcohol, isopulegol, ⁇ -lupulene , ⁇ -myrcene, limonene, neroliol, linalool and/or ⁇ -terpinene.
  • the obtained volatile oil of hemp has a special aroma of hemp.
  • the cannabis flower leaf used in step 1) is the cannabis flower leaf that has not been subjected to the extraction treatment of cannabidiol substances, for example, the volatile oil is extracted before the cannabinol substances are extracted.
  • the dry dehydration is, for example, shade drying; preferably, in step 1), the dry dehydration is performed at a temperature of 10-30°C.
  • the hemp used in the present invention is preferably industrial hemp, that is, industrial hemp flowers and leaves are used to extract the volatile oil.
  • the pulverized powder is coarse powder pulverized into 10-20 mesh (for example, 10 mesh, 13 mesh, 15 mesh, 18 mesh, 20 mesh, etc.), which facilitates the volatilization of volatile components, and It is more convenient to extract cannabidiol components later.
  • 10-20 mesh for example, 10 mesh, 13 mesh, 15 mesh, 18 mesh, 20 mesh, etc.
  • the hemp flower and leaf material is heated in the heating and drying device at 100-120°C for 30-120 min (for example, 30 min, 60 min, 100 min, 120 min, etc.).
  • the heating and drying device is preferably a thermal circulation dryer (or called a hot air circulation dryer) or a belt dryer, preferably these two types of heating and drying devices, which are beneficial to hemp flower and leaf materials
  • the cannabinol components are extracted to reduce the influence on the cannabinol components.
  • the condensing device includes a condenser tube connected to the air outlet of the heating and drying device, and the temperature of the condenser tube is controlled to be -5°C to 5°C (for example, -5°C, -2°C, 0°C, 3°C). °C, 5°C, etc.), the volatile oil storage tank is connected under the condenser; the volatile oil storage tank has an external insulation layer, and the temperature of the insulation layer is controlled at 2-10°C (for example, 2°C, 5°C, 7°C, 10°C, etc.) , Can prevent the volatile oil paste after condensation from continuing to volatilize, and achieve the effect of cold storage. In the volatile oil storage tank, a volatile oil condensate is finally obtained, that is, a volatile oil paste.
  • a volatile oil condensate is finally obtained, that is, a volatile oil paste.
  • the ratio of the mass of the cannabis flower leaf before drying and dehydration in step 1) to the volume of the extractant used in a single extraction in step 4) is 10:1 to 1:1 (for example, 10:1, 7 :1, 5:1, 3:1, 1:1, etc.), the unit is kg/L; preferably, the extraction is performed twice or more in step 4).
  • the volume ratio of the water used for washing in step 5) and the extractant used in step 4) is 10:1 to 1:5. Washing with water can dissolve water-soluble impurities to In the water layer, the terpene components are purified; preferably, the step 5) is washed two or more times.
  • step 5 the distillation is carried out at a temperature of ⁇ 60°C (preferably 40-60°C) and a pressure of -0.02 to -0.05 MPa; preferably, the end point of the distillation is that the outflow rate of the distillate is low At 10 drops/min.
  • the present invention also provides a method for extracting phenolic substances and volatile oil from cannabis, using hemp flower and leaves as a raw material to extract the volatile oil before extracting the phenolic substances, and the volatile oil is extracted by the method described above get on.
  • the phenolic substances refer to cannabidiol, cannabidiol, cannabidiol, cannabidiol, cannabidiol, and/or cannabidiol, etc. contained in cannabis, and the process for extracting cannabidiol substances from cannabis can be adopted The existing processes in this field are carried out, and this will not be repeated.
  • the method of the present invention can prevent the volatile oil of hemp from being discharged together with the exhaust gas during the process of extracting cannabidiol substances from hemp flowers and leaves, and fail to be effectively utilized, resulting in great waste.
  • the present invention also provides a volatile oil, which is obtained by the method described above.
  • the present invention also provides applications of the volatile oil, which can be used in the fields of cigarettes, food, medicine or daily chemicals.
  • the volatile oil can be effectively extracted, and the terpene components in the volatile oil of hemp can be extracted to a greater extent.
  • the residual organic solvent is low (the residual organic solvent is less than 200ppm), and the essential oil can be reduced.
  • Cannabis has a unique aroma; after the volatile oil is extracted from the cannabis flowers and leaves by using the method of the present invention, the cannabinoids can be continuously extracted from the cannabis flowers and leaves.
  • Using the method of the present invention to process cannabis flowers and leaves can prevent the volatile oil from being discharged together with the exhaust gas and failing to be effectively utilized; while in the prior art, when extracting cannabinol substances, the volatile oil (terpene components) is caused by high temperature. , Discharged together with the exhaust gas, resulting in a great waste.
  • Figures 1 to 3 are respectively the total ion current diagrams of the volatile oil of hemp in Examples 1-3.
  • chromatographic column is DB5, (30.0m ⁇ 200 ⁇ m, 0.25 ⁇ m); split ratio, 20:1; inlet temperature is 250°C; starting temperature is 50°C (maintain 1min), with 4°C/min The speed was increased to 210°C (hold for 5 min).
  • Mass spectrometry conditions EI source, electron energy 70eV, ion source 210°C, mass spectrometer: Finniqan ITD800, solvent delay 5min, scanning mass range 40 ⁇ 400u, electron energy 70eV.
  • the hemp mosaics used in the following embodiments are all industrial hemp mosaics.
  • step 2) The hemp flower leaves obtained in step 1) are beaten into coarse powder (20 mesh), and the wrapped hemp seeds are removed by winnowing;
  • step 2) Place the coarse powder obtained in step 2) in a thermal cycle dryer (ie, hot air circulation dryer), and heat at 100°C for 1 hour; the air outlet of the thermal cycle dryer is connected to the condenser tube, and the condenser tube temperature is -5°C; the condenser tube
  • the volatile oil storage tank is connected below, and the volatile oil storage tank is outside the insulation layer, and the temperature of the insulation layer is 5°C; the condensate paste is collected in the volatile oil storage tank;
  • step 4) Wash twice with the same amount of purified water with ethyl acetate, and distill the ethyl acetate layer (60°C, pressure -0.05MPa) and lower than 10 drops/min, which is the end of distillation. Volatile oil.
  • the taste of the obtained volatile oil of hemp it has a special aroma of hemp.
  • P-cymene (1) ⁇ -bisabolol (2), ocimene (3), ⁇ -terpinene (4), ⁇ -caryophyllene (5), guaiacol (6), geraniol Alcohol (7), ⁇ -Pinene (8), ⁇ -Ocimene (9), Terpinolene (10), ⁇ -Pinene (11), Trans-Nerol (12), 4- Methoxybenzyl alcohol (13), isopulegol (14), ⁇ -lupulene (15), ⁇ -myrcene (16), limonene (17), nerolidol (18), linalool (19), ⁇ -terpinene (20).
  • step 2) The hemp flower leaves obtained in step 1) are beaten into coarse powder (10 mesh), and the wrapped hemp seeds are removed by winnowing;
  • step 3 Place the coarse powder obtained in step 2) in a thermal cycle dryer and heat it at 120°C for 2 hours; the air outlet of the thermal cycle dryer is connected to the condenser tube with a temperature of 5°C; the condenser tube is connected to a volatile oil storage tank for volatile oil storage Insulation layer outside the tank, the temperature of the insulation layer is 10°C; condensate paste is collected in the volatile oil storage tank;
  • step 5 Add the same amount of purified water as step 4) to wash twice, and distill the ethyl acetate layer (40°C, pressure -0.02MPa). The end point of distillation is less than 10 drops/min to obtain hemp volatile oil .
  • the taste of the obtained volatile oil of hemp it has a special aroma of hemp.
  • GC-MS can detect the following characteristic components (detection limit 10ppm):
  • P-cymene (1) ⁇ -bisabolol (2), ocimene (3), ⁇ -terpinene (4), ⁇ -caryophyllene (5), guaiacol (6), geraniol Alcohol (7), ⁇ -pinene (8), ⁇ -ocirene (9), terpinene (10), ⁇ -pinene (11), trans-neryl alcohol (12), 4- Methoxybenzyl alcohol (13), isopulegol (14), ⁇ -lupulene (15), ⁇ -myrcene (16), limonene (17), nerolidol (18), linalool (19), ⁇ -terpinene (20).
  • step 2) The hemp flower leaves obtained in step 1) are beaten into coarse powder (20 mesh), and the wrapped hemp seeds are removed by winnowing;
  • step 3 Place the coarse powder obtained in step 2) in a thermal cycle dryer and heat at 110°C for 1 hour; the air outlet of the thermal cycle dryer is connected to the condenser tube with a temperature of 5°C; the condenser tube is connected to a volatile oil storage tank for volatile oil storage Insulation layer outside the tank, the temperature of the insulation layer is 2°C; condensate paste is collected in the volatile oil storage tank;
  • step 5 Add the same amount of purified water as the n-heptane used in step 4) and wash twice, distill the n-heptane layer (35°C, pressure -0.02MPa), and the end point of the distillation is less than 10 drops/min to obtain hemp Volatile oil.
  • the taste of the obtained volatile oil of hemp it has a special aroma of hemp.
  • GC-MS can detect the following characteristic components (detection limit 10ppm):
  • P-cymene (1) ⁇ -bisabolol (2), ocimene (3), ⁇ -terpinene (4), ⁇ -caryophyllene (5), guaiacol (6), geraniol Alcohol (7), ⁇ -pinene (8), ⁇ -ocirene (9), terpinene (10), ⁇ -pinene (11), trans-neryl alcohol (12), 4- Methoxybenzyl alcohol (13), isopulegol (14), ⁇ -lupulene (15), ⁇ -myrcene (16), limonene (17), nerolidol (18), linalool (19), ⁇ -terpinene (20).
  • Chromatographic conditions and system suitability test a capillary column with 100% dimethyl polysiloxane (or similar polarity) as the stationary liquid is used as the chromatographic column; the starting temperature is 40 °C, keep for 6 minutes, and then 10 per minute The temperature is increased to 120°C at a rate of °C; the temperature of the injection port is 200°C; the temperature of the detector is 250°C; the equilibrium temperature of the headspace bottle is 90°C, and the equilibrium time is 30 minutes. Take the reference solution for headspace injection; take 4ml of methanol for the blank sample and add it precisely to the headspace bottle as a blank control.
  • Reference solution Take about 300mg of the extracted organic solvent, accurately weigh it, place it in a volumetric flask, dilute with chromatographic methanol to make the volume 1000ml, accurately measure 4ml, place it in the headspace bottle, and seal it as the reference solution.
  • test solution Take the cannabis volatile oil obtained in each example as the product (about 200 mg), accurately weigh it, place it in a headspace bottle, and accurately add 4 ml of chromatographic methanol solution to seal and dissolve it as the test solution.
  • Determination method Take the reference substance solution and the test substance solution separately, record the chromatogram, and calculate the peak area according to the external standard method. The results are shown in the following table:
  • the method of the present invention can extract terpene components in hemp volatile oil from hemp flowers and leaves, with low organic solvent residue, simple process for extracting hemp volatile oil, and less organic solvents.
  • Using the method of the present invention to treat hemp mosaics can prevent the volatile oil from being discharged with the exhaust gas and fail to be effectively used; on the other hand, after the volatile oil is extracted from the hemp mosaics by the method of the present invention, it can also treat Mosaic continues to extract cannabidiol substances to realize the deep processing and utilization of hemp mosaic.

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Abstract

一种从大麻中提取挥发油的方法，包括如下步骤：1)将大麻花叶干燥脱水；2)将步骤1)干燥脱水后的大麻花叶打成粉，并去掉其中的大麻籽；3)将步骤2)处理后的大麻花叶物料置于加热干燥装置中；该加热干燥装置的出风口与冷凝装置连接，该冷凝装置对该出风口排出的气体进行冷凝处理并获得含挥发油的冷凝物；4)将步骤3)得到的冷凝物用萃取剂进行萃取并取上清液；5)将步骤4)所得上清液用水洗涤并去掉水层，将得到的有机层进行蒸馏。该方法能解决现有技术中大麻的挥发油成分没有得到利用，而是随废气一起排放掉的技术弊端。此外提供了利用该方法从大麻中提取的挥发油及其应用。

Description

一种从大麻中提取挥发油的方法及挥发油的应用 技术领域
本发明涉及烟草、食品领域，特别涉及一种从大麻中提取挥发油的方法。
背景技术
工业大麻化学成分非常复杂，主要包括类脂物、黄酮类化合物、萜烯、碳氢化合物、非环形大苯酚、生物碱、柠檬酸银和环形大麻酚等。人类吸食大麻的历史长达千余年，其中大麻特殊香气主要来自于萜烯类成分，大麻中的萜烯类成分可做为香烟的香料、食品香料使用，具有极高的经济价值；但其挥发性强，目前在制备其他活性物质(例如大麻酚类物质)时，萜烯类成分往往被直接排掉，造成了极大的资源浪费。
发明内容
有鉴于此，本发明提供一种从大麻中提取挥发油的方法，采用本发明的方法，能解决现有技术中大麻的挥发油成分没有得到利用，而是随废气一起排放掉的技术弊端；且采用本发明的方法，所需有机溶剂少，有机溶剂残留低。得到的挥发油具有大麻特有的香气。
本发明为达到其目的，提供如下技术方案：
一种从大麻中提取挥发油的方法，包括如下步骤：
1)将大麻花叶干燥脱水，使大麻花叶的水分含量为20wt％-30wt％，例如20wt％、22wt％、24wt％、26wt％、30wt％等；
2)将步骤1)干燥脱水后的大麻花叶打成粉，并去掉其中的大麻籽，例如通过风选去掉包裹的大麻籽；
3)将步骤2)处理后的大麻花叶物料置于加热干燥装置中，加热温度为100-120℃(例如100℃、105℃、110℃、115℃、120℃等)；所述加热干燥装置的出风口与冷凝装置连接，所述冷凝装置对所述出风口排 出的气体进行冷凝处理并获得含挥发油的冷凝物；
4)将步骤3)得到的冷凝物用萃取剂萃取其中的挥发油，并取上清液，所述萃取剂优选选自乙酸乙酯、正庚烷、正丁醇、正己烷、二氯甲烷、石油醚中的一种或两种以上的组合，采用优选的萃取剂，挥发油收率高，能更好的溶解萜烯类成分；
5)将步骤4)所得上清液用水洗涤并去掉水层，将得到的有机层进行蒸馏，得到大麻挥发油。
本发明的方法中，步骤1)中，将大麻花叶水分控制在20wt％-30wt％，利于步骤3)中挥发油的带出，提高挥发油提取率；而若水分含量太低，将会使挥发油在后续加热干燥时不容易被带出；而若水分含量太高，将由于物料过湿而导致能耗增加。步骤3)中，在100-120℃下进行加热干燥，一方面在该温度能使挥发油类成分95％以上挥发；另一方面能使大麻酚酸类成分进行脱羧反应，利于后续大麻酚类物质的后续提取工艺的进行，能增加大麻酚类成分的收率。经本发明的方法得到的大麻挥发油主要成分为萜烯类，特征成分例如含对伞花烃、α-没药醇、罗勒烯、α-松油烯、β-石竹烯、愈创木醇、香叶醇、β-蒎烯、β-罗勒烯、异松油烯、β-蒎烯、反式-橙花叔醇、4-甲氧基苯甲醇、异胡薄荷醇、α-蛇麻烯、β-月桂烯、柠檬烯、橙花叔醇、芳樟醇和/或γ-松油烯等。所得的大麻挥发油具有大麻特殊香气。
本发明中，步骤1)所用的大麻花叶为未经过大麻酚类物质提取处理的大麻花叶，例如在大麻酚类物质提取之前，进行挥发油提取。
步骤1)中，所述干燥脱水例如为阴干；优选的，步骤1)中，所述干燥脱水在10-30℃的温度条件下进行。本发明所用的大麻优选为工业大麻，即采用工业大麻花叶来提取挥发油。
优选的，步骤2)中，所述打成粉为打成10-20目(例如10目、13目、15目、18目、20目等)的粗粉，利于挥发性成分的挥发，而且更方便后期提取大麻酚类成分。
一些优选实施方式中，步骤3)中，所述大麻花叶物料在所述加热干燥装置中于100-120℃加热30-120min(例如30min、60min、100min、 120min等)。一些优选实施方式中，步骤3)中，所述加热干燥装置优选为热循环干燥器(或称为热风循环干燥器)或带式干燥器，优选这两类加热干燥装置，利于大麻花叶物料在进行挥发油提取后，进行大麻酚类成分的提取，减少对大麻酚类成分的影响。
一些优选实施方式中，所述冷凝装置包括与加热干燥装置的出风口相连接的冷凝管，冷凝管的温度控制为-5℃至5℃(例如-5℃、-2℃、0℃、3℃、5℃等)，冷凝管下接挥发油储罐；所述挥发油储罐外设保温层，保温层的温度控制为2-10℃(例如2℃、5℃、7℃、10℃等)，能防止冷凝后的挥发油膏体继续挥发，达到冷藏保存的效果。在挥发油储罐中最终得到挥发油冷凝膏，即挥发油膏状物。
一些优选实施方式中，步骤1)中干燥脱水前的大麻花叶质量与步骤4)中萃取时单次萃取所用萃取剂的体积之比为10:1-1:1(例如10:1、7:1、5:1、3:1、1:1等)，单位为kg/L；优选的，步骤4)中萃取两次或多次。
一些优选实施方式中，步骤5)中进行所述洗涤所用的水与步骤4)中所用萃取剂的体积比为10:1-1:5，用水进行洗涤，能将溶于水的杂质溶解到水层，纯化萜烯类成分；优选的，步骤5)中洗涤两次或多次。
一些优选实施方式中，步骤5)中，所述蒸馏在温度＜60℃(优选40-60℃)，压强为-0.02至-0.05MPa条件下进行；优选蒸馏终点为馏出液的流出速度低于10滴/分。
本发明还提供一种从大麻中提取酚类物质和挥发油的方法，以大麻花叶为原料，在进行提取酚类物质之前先提取所述挥发油，所述挥发油的提取采用上文所述的方法进行。所述酚类物质是指大麻中含有的大麻二酚、次大麻二酚、大麻萜酚、次四氢大麻酚和/或大麻环萜酚等，从大麻中提取大麻酚类物质的工艺可采用本领域现有工艺进行，对此不作赘述。采用本发明的方法可以避免大麻挥发油在大麻花叶提取大麻酚类物质过程中随废气一同排出，而未能得到有效利用，造成极大浪费。
本发明还提供一种挥发油，该挥发油采用上文所述的方法获得。
本发明还提供所述挥发油的应用，所述挥发油能应用于香烟、食品、药品或日化品领域。
本发明提供的技术方案具有如下有益效果：
采用本发明的方法，能有效的提取得到其中的挥发油，较大限度的提取大麻挥发油中的萜烯类成分，有机溶剂残留低(有机溶剂残留在200ppm以下)，将其制成香精油能还原大麻特有香气；采用本发明方法从大麻花叶中提取得到挥发油后，还可对大麻花叶继续进行大麻酚类物质的提取。
利用本发明的方法来处理大麻花叶，可避免其中的挥发油随废气一同排出而未能得到有效利用；而现有技术中在提取大麻酚类物质时，挥发油(萜烯类成分)由于高温作用，随废气一起排放掉，造成了极大的浪费。
附图说明
图1-图3，依次分别是实施例1-3的大麻挥发油总离子流图。
具体实施方式
为了更好的理解本发明的技术方案，下面结合实施例进一步阐述本发明的内容，但本发明的内容并不仅仅局限于以下实施例。
以下实施例中涉及的GC-MS检测，说明如下：
气相色谱条件：色谱柱为DB5，(30.0m×200μm，0.25μm)；分流比，20:1；进样口温度为250℃；起始温度50℃(保持1min)，以4℃/min的速度升至210℃(保持5min)。
质谱条件：EI源，电子能量70eV，离子源210℃，质谱仪：Finniqan ITD800，溶剂延迟为5min，扫描质量范围40～400u，电子能量70eV。
以下各个实施例所用的大麻花叶均为工业大麻花叶。
实施例1
1)取新鲜大麻花叶100kg，30℃阴凉干燥72h，大麻花叶水分含量 为21wt％；
2)将步骤1)得到的大麻花叶打成粗粉(20目)，风选去掉包裹的大麻籽；
3)将步骤2)得到的粗粉置于热循环干燥器(即热风循环干燥器)，100℃加热1h；热循环干燥器的出风口与冷凝管连接，冷凝管温度-5℃；冷凝管下接挥发油储罐，挥发油储罐外设保温层，保温层温度为5℃；在挥发油储罐中收集得到冷凝膏；
4)冷凝膏加乙酸乙酯萃取两次，每次乙酸乙酯用量为100L，合并上清液；
5)加与步骤4)乙酸乙酯用量为等量的纯化水洗涤两次，将乙酸乙酯层进行蒸馏(60℃，压强-0.05MPa)低于10滴/分即为蒸馏终点，得大麻挥发油。
所得大麻挥发油的味觉：具有大麻特殊香气。
鉴别：通过GC-MS检测能够检测到如下特征性成分(检测限10ppm)，
对伞花烃(1)、α-没药醇(2)、罗勒烯(3)、α-松油烯(4)、β-石竹烯(5)、愈创木醇(6)、香叶醇(7)、α-蒎烯(8)、β-罗勒烯(9)、异松油烯(10)、β-蒎烯(11)、反式-橙花叔醇(12)、4-甲氧基苯甲醇(13)、异胡薄荷醇(14)、α-蛇麻烯(15)、β-月桂烯(16)、柠檬烯(17)、橙花叔醇(18)、芳樟醇(19)、γ-松油烯(20)。
大麻挥发油总离子流图参见图1，各特征峰信息如下表所述：
峰序号 保留时间 鉴别成分
1 20.8431 对伞花烃
2 24.6419 α-没药醇
3 36.2232 罗勒烯
4 36.4626 α-松油烯
5 37.4119 β-石竹烯
6 38.4571 愈创木醇
7 38.7662 香叶醇
8 41.239 α-蒎烯
9 41.3389 β-罗勒烯
10 41.6722 异松油烯
11 42.6882 β-蒎烯
12 44.7024 反式-橙花叔醇
13 45.3459 4-甲氧基苯甲醇
14 47.0311 异胡薄荷醇
15 48.2081 α-蛇麻烯
16 49.1931 β-月桂烯
17 51.4322 柠檬烯
18 52.1775 橙花叔醇
19 55.3664 芳樟醇
20 55.7843 γ-松油烯
实施例2：
1)取新鲜大麻花叶10kg,24℃阴凉干燥36h，大麻花叶水分含量为25wt％；
2)将步骤1)得到的大麻花叶打成粗粉(10目)，风选去掉包裹的大麻籽；
3)将步骤2)得到的粗粉置于热循环干燥器，120℃加热2h；热循环干燥器的出风口与冷凝管连接，冷凝管温度5℃；冷凝管下接挥发油储罐，挥发油储罐外设保温层，保温层温度为10℃；在挥发油储罐中收集得到冷凝膏；
4)冷凝膏加正己烷萃取两次，每次乙酸乙酯用量为1L，合并上清液；
5)加与步骤4)正己烷用量等量的纯化水洗涤两次，将乙酸乙酯层进行蒸馏(40℃，压强-0.02MPa)，低于10滴/分即为蒸馏终点，得大麻挥发油。
所得大麻挥发油的味觉：具有大麻特殊香气。
鉴别：通过GC-MS检测能够检测到如下特征性成分(检测限10ppm)：
对伞花烃(1)、α-没药醇(2)、罗勒烯(3)、α-松油烯(4)、β-石竹烯(5)、愈创木醇(6)、香叶醇(7)、β-蒎烯(8)、β-罗勒烯(9)、异松油烯(10)、β-蒎烯(11)、反式-橙花叔醇(12)、4-甲氧基苯甲醇(13)、异胡薄荷醇(14)、α-蛇麻烯(15)、β-月桂烯(16)、柠檬烯(17)、橙花叔醇(18)、芳樟醇(19)、γ-松油烯(20)。
大麻挥发油总离子流图参见图2，各特征峰信息如下表所示：
峰序号 保留时间 鉴别成分
1 20.9116 对伞花烃
2 24.7314 α-没药醇
3 36.3321 罗勒烯
4 36.4871 α-松油烯
5 37.3965 β-石竹烯
6 38.6019 愈创木醇
7 38.7381 香叶醇
8 41.1098 α-蒎烯
9 41.2661 β-罗勒烯
10 41.7221 异松油烯
11 42.6577 β-蒎烯
12 44.7143 反式-橙花叔醇
13 45.4013 4-甲氧基苯甲醇
14 47.1479 异胡薄荷醇
15 48.1934 α-蛇麻烯
16 49.2155 β-月桂烯
17 51.4335 柠檬烯
18 52.1972 橙花叔醇
19 55.4789 芳樟醇
20 55.7553 γ-松油烯
实施例3：
1)取新鲜大麻花叶10kg,10℃阴凉干燥48h，大麻花叶水分含量为28wt％；
2)将步骤1)得到的大麻花叶打成粗粉(20目)，风选去掉包裹的大麻籽；
3)将步骤2)得到的粗粉置于热循环干燥器，110℃加热1h；热循环干燥器的出风口与冷凝管连接，冷凝管温度5℃；冷凝管下接挥发油储罐，挥发油储罐外设保温层，保温层温度为2℃；在挥发油储罐中收集得到冷凝膏；
4)冷凝膏加正庚烷萃取两次，每次正庚烷用量为5L，合并上清液；
5)加与步骤4)所用正庚烷等量的纯化水洗涤两次，将正庚烷层进行蒸馏(35℃，压强-0.02MPa)，低于10滴/分即为蒸馏终点，得大麻挥发油。
所得大麻挥发油的味觉：具有大麻特殊香气。
鉴别：通过GC-MS检测能够检测到如下特征性成分(检测限10ppm)：
对伞花烃(1)、α-没药醇(2)、罗勒烯(3)、α-松油烯(4)、β-石竹烯(5)、愈创木醇(6)、香叶醇(7)、β-蒎烯(8)、β-罗勒烯(9)、异松油烯(10)、β-蒎烯(11)、反式-橙花叔醇(12)、4-甲氧基苯甲醇(13)、异胡薄荷醇(14)、α-蛇麻烯(15)、β-月桂烯(16)、柠檬烯(17)、橙花叔醇(18)、芳樟醇(19)、γ-松油烯(20)。
大麻挥发油总离子流图参见图3，各特征峰信息如下表所示：
峰序号 保留时间 鉴别成分
1 20.9432 对伞花烃
2 24.7224 α-没药醇
3 36.4531 罗勒烯
4 36.4792 α-松油烯
5 37.3744 β-石竹烯
6 38.6124 愈创木醇
7 38.6973 香叶醇
8 41.1266 α-蒎烯
9 41.2983 β-罗勒烯
10 41.8123 异松油烯
11 42.6206 β-蒎烯
12 44.6868 反式-橙花叔醇
13 45.4349 4-甲氧基苯甲醇
14 47.0987 异胡薄荷醇
15 48.1647 α-蛇麻烯
16 49.1984 β-月桂烯
17 51.4172 柠檬烯
18 52.3391 橙花叔醇
19 55.3077 芳樟醇
20 55.6289 γ-松油烯
实施例4
对上述各个实施例的残留溶剂进行检测：
色谱条件与系统适用性试验：以100％二甲基聚硅氧烷(或极性相近)为固定液的毛细管柱为色谱柱；起始温度为40℃，保持6分钟，再以每分钟10℃的速率升温至120℃；进样口温度为200℃；检测器温度为250℃；顶空瓶平衡温度为90℃，平衡时间为30分钟。取对照品溶液顶空进样；空白样取甲醇4ml，精密加入顶空瓶中，作为空白对照。
对照品溶液：取萃取有机溶剂约300mg，精密称定，置容量瓶中，用色谱甲醇稀释定容至1000ml，精密量取4ml，置顶空瓶中，密封，作为对照品溶液。
供试品溶液的制备：分别取各实施例所得到大麻挥发油作为本品(约 200mg)，精密称定，置顶空瓶中，精密加入色谱甲醇溶液4ml密封使溶解，作为供试品溶液。
测定法：取对照品溶液和供试品溶液分别进样，记录色谱图，按外标法以峰面积计算，结果见如下表：
Figure PCTCN2020078031-appb-000001
综上可见，采用本发明的方法，能从大麻花叶中提取得到大麻挥发油中的萜烯类成分，且有机溶剂残留低，提取大麻挥发油的工艺简单，所需有机溶剂少。利用本发明的方法来处理大麻花叶，一方面可避免其中的挥发油随废气一同排出而未能得到有效利用；另一方面采用本发明方法从大麻花叶中提取得到挥发油后，还可对大麻花叶继续进行大麻酚类物质的提取，实现大麻花叶的深度加工利用。
本领域技术人员可以理解，在本说明书的教导之下，可对本发明做出一些修改或调整。这些修改或调整也应当在本发明权利要求所限定的范围之内。

Claims (10)

  1. 一种从大麻中提取挥发油的方法，其特征在于，包括如下步骤：
    1)将大麻花叶干燥脱水，使大麻花叶的水分含量为20wt％-30wt％；
    2)将步骤1)干燥脱水后的大麻花叶打成粉，并去掉其中的大麻籽；
    3)将步骤2)处理后的大麻花叶物料置于加热干燥装置中，加热温度为100-120℃；所述加热干燥装置的出风口与冷凝装置连接，所述冷凝装置对所述出风口排出的气体进行冷凝处理并获得含挥发油的冷凝物；
    4)将步骤3)得到的冷凝物用萃取剂萃取其中的挥发油，取上清液，所述萃取剂优选选自乙酸乙酯、正庚烷、正丁醇、正己烷、二氯甲烷、石油醚中的一种或两种以上的组合；
    5)将步骤4)所得上清液用水洗涤并去掉水层，将得到的有机层进行蒸馏，得到大麻挥发油。
  2. 根据权利要求1所述的方法，其特征在于，步骤1)所用的大麻花叶为未经过大麻酚类物质提取处理的大麻花叶，所述大麻优选为工业大麻。
  3. 根据权利要求1或2所述的方法，其特征在于，步骤1)中，所述干燥脱水在10-30℃的温度条件下进行；
    和/或，步骤2)中，所述打成粉为打成10-20目的粗粉。
  4. 根据权利要求1-3任一项所述的方法，其特征在于，步骤3)中，所述大麻花叶物料在所述加热干燥装置中于100-120℃加热30-120min，所述加热干燥装置优选为热循环干燥器或带式干燥器。
  5. 根据权利要求1-4任一项所述的方法，其特征在于，所述冷凝装置包括与加热干燥装置的出风口相连接的冷凝管，冷凝管的温度控制为-5℃至5℃，冷凝管下接挥发油储罐，所述挥发油储罐外设保温层，保温层的温度控制为2-10℃。
  6. 根据权利要求1-5任一项所述的方法，其特征在于，步骤1)中干燥脱水前的大麻花叶质量与步骤4)中萃取时单次萃取所用萃取剂的体积之比为10:1-1:1，单位为kg/L；优选的，步骤4)中萃取两次或多次；
    优选的，步骤5)中进行所述洗涤所用的水与步骤4)中所用萃取剂的体积比为10:1-1:5；进一步优选的，步骤5)中洗涤两次或多次。
  7. 根据权利要求1-6任一项所述的方法，其特征在于，步骤5)中，所述蒸馏在温度＜60℃，压强为-0.02至-0.05MPa条件下进行；优选所述蒸馏的温度为40-60℃；
    优选蒸馏终点为馏出液的流出速度低于10滴/分。
  8. 一种从大麻中提取酚类物质和挥发油的方法，其特征在于，以大麻花叶为原料，在进行酚类物质提取之前先提取所述挥发油，所述挥发油的提取采用权利要求1-7任一项所述的方法进行。
  9. 一种挥发油，其特征在于，采用权利要求1-8任一项所述的方法获得。
  10. 权利要求9所述的挥发油的应用，其特征在于，所述挥发油应用于香烟、食品、药品或日化品领域。
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