WO2022166301A1 - 一种大麻除杂方法 - Google Patents

一种大麻除杂方法 Download PDF

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WO2022166301A1
WO2022166301A1 PCT/CN2021/131077 CN2021131077W WO2022166301A1 WO 2022166301 A1 WO2022166301 A1 WO 2022166301A1 CN 2021131077 W CN2021131077 W CN 2021131077W WO 2022166301 A1 WO2022166301 A1 WO 2022166301A1
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extract
cannabis
organic solvent
extraction
impurity removal
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PCT/CN2021/131077
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French (fr)
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叶彬
田汉玉
罗飞
柴岩岩
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浙江双子智能装备有限公司
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Publication of WO2022166301A1 publication Critical patent/WO2022166301A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/86—Purification; separation; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
    • C07C39/23—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring polycyclic, containing six-membered aromatic rings and other rings, with unsaturation outside the aromatic rings

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  • the present application relates to the field of cannabis impurity removal, more specifically, it relates to a cannabis impurity removal method.
  • cannabidiol compounds are the main active components in cannabis plants, mainly including tetrahydrocannabinol (THC), cannabidiol (CBN), cannabidiol (CBD), cannabidiol (CBG), cannabidiol (CBC) etc., of which THC, cannabidiol and cannabidiol account for more than 90% of cannabidiol compounds.
  • cannabidiol not only has no neurotoxicity, but also has significant medicinal value; relevant pharmacological studies have shown that it can hinder the effect of tetrahydrocannabinol on the human nervous system, and has antispasmodic, anti-rheumatoid arthritis, Anti-anxiety and other pharmacological activities have huge industrial development value.
  • the process of extracting cannabidiol from cannabis mainly includes two parts: impurity removal and refining.
  • impurity removal will directly affect the effect of subsequent refining.
  • a good impurity removal method can reduce the pressure and cost of refining.
  • the impurity removal processes are column chromatography and membrane filtration.
  • Running costs become high and efficiency is low.
  • Membrane filtration and impurity removal membrane equipment is expensive and has high operation and maintenance costs, making it difficult to be widely used. To sum up, the impurity removal method cannot take into account the cost and the effect of impurity removal.
  • the present application provides a method for removing impurities from cannabis.
  • a hemp impurity removal method comprising the following steps:
  • S1 pretreatment: drying and pulverizing the cannabis leaves to obtain raw material powder; extracting the raw material powder with an ethanol solution to obtain a cannabis extract;
  • the organic solvent is at least one of alkanes or halogenated hydrocarbons.
  • the cannabis is processed into a cannabis extract by pretreatment, which is convenient for subsequent impurity removal treatment.
  • Winterization is a method of crystallization and separation. By cooling, glycerides with a higher freezing point are crystallized out, and impurities such as wax and solid fat in the cannabis extract are separated.
  • the extract contains cannabidiol (CBD), cannabidiol (CBG), cannabidiol (CBC), cannabidiol (CBN), tetrahydrocannabinol (THC) and other unique substances contained in cannabis plants With some impurities; decarboxylation will remove carbon dioxide from the carboxyl group, and convert cannabidiol, tetrahydrocannabinol, cannabidiol, cannabidiol, and cannabidiol into cannabidiol and tetrahydrocannabinol, respectively.
  • CBD cannabidiol
  • CBD cannabidiol
  • CBD cannabidiol
  • CBD cannabidiol
  • CBD cannabidiol
  • CBN cannabidiol
  • THC tetrahydrocannabinol
  • cannabidiol, cannabidiol, cannabidiol to improve the yield of the final product; at the same time, some organic compounds will be carbonized to produce impurities. Then, the CBD in the extract is dissolved and brought out through the organic solvent, and most of the impurities are removed to complete the removal of impurities.
  • the organic solvent is at least one of chloroform, n-hexane, n-heptane and n-octane.
  • organic solvents chloroform, n-hexane, n-heptane and n-octane have strong practicability, are stable and non-volatile at operating temperature, have moderate boiling point, and have low energy consumption for recovery, which is convenient for complete removal; The cost is reasonable, and it is not toxic.
  • organic solvents can be mixed and used, but it will increase the difficulty of recycling.
  • the temperature of the organic solvent extraction is 50-90°C.
  • the volume ratio of the quality of the extract to the organic solvent is 1:5-1:15.
  • the organic solvent is added in 2-4 times.
  • step S4 stirring is continued during extraction.
  • the cannabis extract is concentrated to a cannabidiol content of 1-5% and then winterized.
  • concentration is used to complete the removal of impurities from cannabis, so as to achieve the effects of simple operation and reduced cost input, and simultaneously improve the quality of the final product. And avoid the problems of environmental pollution caused by waste fillers.
  • At least one of chloroform, n-hexane, n-heptane and n-octane is preferably used as the organic solvent, which has strong practicability, low energy consumption for recovery and moderate cost.
  • the extraction temperature and time and the amount of organic solvent are preferred, so as to obtain faster extraction speed and better extraction effect.
  • Fig. 1 is the liquid chromatogram of the extract after S3 step of embodiment 22;
  • Fig. 2 is the liquid chromatogram of the cannabis extract obtained after step S5 in Example 22.
  • Embodiment 1 a kind of hemp impurity removal method, may further comprise the steps:
  • the cannabis extract added with ethanol aqueous solution is placed at a temperature of -50 ° C for 24 hours, and then transferred to a plate-and-frame filter press equipment for filtration to remove impurities to obtain a filtrate;
  • the organic solvent is dichloromethane, and the mass ratio of the extract to the volume of the organic solvent is 1:1; the filter aid is activated carbon and diatomite with a mass ratio of 1:1;
  • S5 transfer the extract to a vacuum concentration device, and concentrate to remove the organic solvent under the pressure of -0.08MPa to obtain a cannabis extract.
  • Embodiment 2 a kind of hemp impurity removal method, the difference with embodiment 1 is:
  • the drying temperature is 150°C, and the drying is performed until the water content is 1%;
  • the extraction temperature of the aqueous ethanol solution is 35°C, and the extraction time is 50min;
  • the heating temperature is 120°C;
  • the organic solvent is n-nonane
  • the extraction temperature is 95°C
  • the extraction time is 30 min
  • the ratio of the extract mass to the organic solvent volume is 1:10.
  • the amount of filter aid used is 20% of the quality of the extract, and the filter aid is diatomaceous earth.
  • Embodiment 3 a kind of hemp impurity removal method, the difference with embodiment 1 is:
  • the drying temperature is 120°C, and the drying is performed until the water content is 3%;
  • the extraction temperature of the ethanol aqueous solution is 15°C, and the extraction time is 75min;
  • the heating temperature is 150°C;
  • the organic solvent is composed of chloroform and n-nonane with a mass ratio of 1:1, the extraction temperature is 45°C, the extraction time is 40min, and the ratio of the extract mass to the organic solvent volume is 1:20.
  • the amount of filter aid used is 10% of the quality of the extract, and the filter aid is activated carbon.
  • Example 4 A method for removing impurities from cannabis, the difference from Example 1 is that the organic solvent is chloroform.
  • Example 5 A method for removing impurities from cannabis, the difference from Example 1 is that the organic solvent is n-heptane.
  • Example 6 A method for removing impurities from cannabis, the difference from Example 1 is that the organic solvent is composed of chloroform, n-hexane and n-heptane with a mass ratio of 1:1:1.
  • Example 7 A method for removing impurities from cannabis, the difference from Example 5 is that the extraction temperature is 50°C.
  • Example 8 A method for removing impurities from cannabis, the difference from Example 5 is that the extraction temperature is 70°C.
  • Example 9 A method for removing impurities from cannabis, the difference from Example 5 is that the extraction temperature is 90°C.
  • Example 10 A method for removing impurities from cannabis, the difference from Example 8 is that the ratio of extract quality to organic solvent volume is 1:5.
  • Example 11 A method for removing impurities from cannabis, the difference from Example 8 is that the ratio of the extract mass to the volume of the organic solvent is 1:10.
  • Example 12 A method for removing impurities from cannabis, the difference from Example 8 is that the ratio of the extract mass to the volume of the organic solvent is 1:15.
  • Example 13 A method for removing impurities from cannabis, the difference from Example 12 is that the number of times of extraction is 2, the organic solvent is divided into two equal parts, one part is added each time, and each extraction time is 40min.
  • Example 14 A method for removing impurities from cannabis, the difference from Example 12 is that the number of extractions is 3 times, the organic solvent is divided into three equal parts, one part is added each time, and each extraction time is 40min.
  • Example 15 A method for removing impurities from cannabis, the difference from Example 12 is that the number of extractions is 4 times, the organic solvent is divided into four parts on average, one part is added each time, and each extraction time is 40min.
  • Example 16 A method for removing impurities from cannabis, the difference from Example 14 is that each extraction time is 5min.
  • Example 17 A method for removing impurities from cannabis, the difference from Example 14 is that each extraction time is 10 min.
  • Example 18 a method for removing impurities from cannabis, the difference from Example 14 is that each extraction time is 30min.
  • Example 19 a method for removing impurities from cannabis, the difference from Example 17 is that stirring is performed during extraction, and the stirring speed is 60 r/min.
  • Example 20 A method for removing impurities from cannabis, the difference from Example 17 is that stirring is performed during extraction, and the stirring speed is 30 r/min.
  • Example 21 A method for removing impurities from cannabis, the difference from Example 19 is that in S2, the concentration of CBD is 1%.
  • Example 22 A method for removing impurities from cannabis, the difference from Example 19 is that in S2, the concentration of CBD is 5%.
  • activated carbon was purchased from Jiangsu Agnes Environmental Technology Co., Ltd.
  • diatomite was purchased from Guangzhou Haozhao Chemical Co., Ltd.
  • Comparative Example 1 a cannabidiol-rich hemp extract and a preparation method thereof.
  • the mature hemp flowers and leaves were spread in a general oven, the temperature was set to 80°C, and the dry heat treatment time was 3 hours.
  • grind it with a pulverizer take 1.5 kg of dried hemp flower leaves, put it in the material tank of the subcritical extraction device, and inject the n-butane containing 40% ethanol in the subcritical state in the solvent tank into the material tank, Extraction was carried out at a temperature of 45° C. and an extraction pressure of 0.6 MPa for 45 minutes. Then desolventized under reduced pressure, the extract was taken out, and the extraction was repeated 3 times.
  • a certain amount of ethanol was added to the obtained ethanol solution containing the extract to make the solid-liquid ratio reach 1:7, and then placed in a -10° C. refrigerator for winterization treatment for 45 minutes. Then, centrifugation was performed for 20 minutes using a centrifuge at -10°C. The rotational speed is 4500 rpm. The supernatant was decolorized by adding activated carbon, and then placed on a shaker with a rotation speed of 150 rpm for 25 minutes. Then, the above mixture is filtered to obtain a filtrate. The filtrate was placed in a rotary evaporation flask, and rotary evaporation was performed under the conditions of a water bath temperature of 50°C and a rotational speed of 50 rev/min to obtain the cannabis extract.
  • Comparative Example 2 The process of extracting dihydrocannabinol (CBD) from industrial hemp.
  • the raw materials are flowers and leaves in full bloom.
  • the flowers and leaves are pre-dried or roasted, and the moisture content is between 10-15%.
  • the lime soil content is below 3%.
  • the raw materials are put into the baking equipment, the temperature is controlled between 130-160° C. (160° C. is selected in this comparative example), and the time is controlled at 15-35 minutes (20 minutes is selected in this comparative example).
  • the second step is to grind the dried flowers and leaves to reach between 5-10 meshes.
  • the third step is to put the ground flowers and leaves into the soaker for soaking, and the soaking solvent is petroleum ether, n-hexane or 6# solvent oil.
  • the soaking temperature is not higher than 50 °C (50 °C is selected in this comparative example), and the soaking time is not less than 1 hour each time (1 h is selected in this comparative example).
  • the soaked mixed solution is filtered through the filter screen in the equipment and then pumped to the concentrator for separation and concentration.
  • the concentration separator is controlled at a temperature between 90 and 120° C. (100° C. is selected for this comparative example).
  • the solid and semi-solid paste obtained after the solvent is evaporated and concentrated is the extract rich in CBD.
  • Comparative Example 3 The difference from Example 1 is that the cannabis extract obtained by S1 is concentrated, concentrated to a CBD content of 8%, and a 95V/V ethanol aqueous solution is added to adjust to an ethanol volume content of 60%, at 60r/min. After stirring for 5 min under the conditions, the decarboxylation of S3 was carried out after winterization treatment, and then put into the vacuum concentration equipment, and concentrated to the extract under the pressure of -0.09MPa.
  • Comparative Example 4 The difference from Example 1 is that the difference from Example 1 is that the cannabis extract obtained by S1 is concentrated, concentrated to a CBD content of 8%, and 95V/V ethanol aqueous solution is added to adjust to the ethanol volume content of 8%. 60%, after stirring for 5min under the condition of 60r/min, put it into the vacuum concentration equipment first, concentrate it to the extract under the pressure of -0.09MPa, and then carry out the decarboxylation treatment in S3.
  • Test subjects Examples 1-22 and Comparative Examples 1-4, a total of 26 test groups.
  • Example 1-22 and Comparative Examples 1-4 were tested by taking materials from the same batch of raw material powder.
  • the extract after completing step S3 is sampled to carry out CBD content detection, and the CBD content in 80g is converted to record the CBD content of the extract before extraction, and the sampling is carried out after step S5 is completed.
  • Comparative Examples 1-4 the finally obtained cannabis extract or extract was tested for CBD content.
  • the original content of CBD is obtained from the detection of CBD content in the hemp extract of Example 1, and the content is 40.2%.
  • the content of CBD was measured using a high-performance liquid chromatograph under the conditions of a column temperature of 30 °C, a mobile phase of 0.4 ml/min, and a wavelength of 210 nm.
  • the CBD standard was purchased from Changsha Yingsheng Biotechnology Co., Ltd.
  • Test results The test results of CBD content and loss rate in Examples 1-22 and Comparative Examples 1-3 are recorded as shown in Table 1.
  • the CBD content of the pre-extraction extracts of the comparative examples and comparative examples 3-4 shows that the pre-extraction processing step parameters and the processing step sequence have an impact on the pre-extraction CBD content, and the pre-extraction steps adopted in this example are effective. Increase the CBD content of the extract before extraction, thereby increasing the final CBD content and improving the effect of cannabis removal.
  • Examples 4-6 limit the composition of the organic solvent
  • Examples 7-9 further limit the extraction temperature on the basis of Example 5, and Examples 10-12 are based on Example 8.
  • the dosage of the organic solvent is further limited, and the CBD content is further increased and the loss rate is reduced.
  • Examples 13-15 increase the extraction times on the basis of Example 12, and greatly improve the CBD content of the extract after extraction on the basis of Example 12, indicating that the parameters of extraction have a great influence on the extraction effect and efficiency.
  • Example The preferred parameters of can bring better extraction effect.
  • Examples 16-18 limit the extraction time each time on the basis of Example 14. It can be seen that the effect of Example 16 is less, but when it reaches 10min each time, the effect is already very good, which can save energy. On the basis of ensuring the extraction effect.
  • Examples 19-20 add stirring on the basis of Example 17, which can further improve the extraction effect and can be widely used; and the increase in stirring is not easy to cause a substantial increase in cost, which is beneficial to control the processing cost.
  • the amount of solvent used and the consumption of resources can be greatly reduced.
  • the method used in this application can reduce the solvent usage by 70%; compared with the membrane filtration method, the equipment cost can be reduced, and the solvent usage can be reduced by 30%.
  • Test object Example 22, a total of 1 group of test samples.
  • Test method use high performance liquid chromatography to detect the CBD components of the extract after step S3 and the cannabis extract obtained in step S5.
  • Test results The test of impurity removal effect is shown in Figure 1 and Figure 2.

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

本申请涉及大麻除杂领域，具体公开了一种大麻除杂方法。一种大麻除杂方法包括以下步骤：S1：预处理：将大麻花、叶烘干、粉碎，得到原料粉；将原料粉用乙醇溶液进行提取，得到大麻提取液；S2：将大麻提取液浓缩至后，进行冬化处理，过滤后得到过滤液，将过滤液的浓缩至浸膏；S3：将浸膏进行脱羧处理；S4：向脱羧后的浸膏中加入有机溶剂进行萃取，过滤后得到萃取液；S5：将萃取液浓缩除去有机溶剂后得到大麻提取物；所述有机溶剂为烷烃类或卤代烃中的至少一种。本申请的制备方法可用于大麻二酚提取中的大麻除杂，其具有成本合适，除杂效果好的优点。

Description

一种大麻除杂方法 技术领域
本申请涉及大麻除杂领域，更具体地说，它涉及一种大麻除杂方法。
背景技术
近年来，随着人们对大麻的不断研究与探索，发现大麻植株含有一类特有的物质，即大麻酚类化合物。大麻酚类化合物是大麻植物中的主要活性成分，主要包括四氢大麻酚(THC)、大麻酚(CBN)、大麻二酚(CBD)、大麻萜酚(CBG)、大麻环萜酚(CBC)等，其中四氢大麻酚、大麻酚和大麻二酚占大麻酚类化合物的90％以上。
其中，大麻二酚不仅不具备神经毒性，而且具有显著的药用价值；相关的药理研究表明，其能阻碍四氢大麻酚对人体神经系统的影响，并具有抗痉挛、抗风湿性关节炎、抗焦虑等药理活性，具有巨大产业开发价值。
近年来，大麻二酚的市场需求日益加大，大量的企业开始关注于工业大麻领域。从大麻中提取大麻二酚的工艺主要包括除杂和精制两大部分，除杂的效果会直接影响到后续精制的效果，效果好的除杂方式可以减小精制的压力和成本消耗。
相关技术中，最常被使用的除杂工艺是柱层析除杂以及膜过滤除杂。单纯通过柱层析法达到除杂的目的需要经过两道甚至多道层析柱，这会导致有效成分的损耗加大，溶剂的耗量加大，填料使用量的增多，最终使得整个工艺的运行成本变高，且效率低。膜过滤除杂的膜设备价格较高，运行维护成本高，难以得到广泛的使用。综上，除杂方法无法兼顾成本和除杂效果。
发明内容
为了兼顾除杂的成本和除杂效果，本申请提供一种大麻除杂方法。
第一方面，本申请提供了如下技术方案：一种大麻除杂方法，包括以下步骤：
S1：预处理：将大麻花叶烘干、粉碎，得到原料粉；将原料粉用乙醇溶液进行提取，得到大麻提取液；
S2：将大麻提取液浓缩之后，进行冬化处理，过滤后得到过滤液，将过滤液浓缩至浸膏；
S3：将浸膏进行脱羧处理；
S4：向脱羧后的浸膏中加入有机溶剂进行萃取，过滤后得到萃取液；
S5：将萃取液浓缩除去有机溶剂后得到大麻提取物；
所述有机溶剂为烷烃类或卤代烃中的至少一种。
通过采用上述技术方案，预处理将大麻处理成大麻提取液，方便后续的除杂处理。冬化是一种晶析分离的方法，通过降温将凝固点较高的甘油酯等结晶析出，将大麻提取液中的蜡质、固体脂肪等杂质分离出来。浓缩后，浸膏中包含大麻二酚(CBD)、大麻萜酚(CBG)、大麻环萜酚(CBC)、大麻酚(CBN)、四氢大麻酚(THC)等大麻植株中含有的特有物质与部分杂质；脱羧处理会将羧基脱去二氧化碳，将大麻二酚酸、四氢大麻酚酸、大麻酚酸、大麻萜酚酸、大麻环萜酚酸分别转化为大麻二酚、四氢大麻酚、大麻酚、大麻萜酚、大麻环萜酚，提高最终产品产率；同时会有部分有机物发生碳化产生杂质。再通过有机溶剂将浸膏中的CBD溶解带出，去除大部分杂质，完成除杂。通过上述步骤，使用有机溶剂萃取分离可以代替原有的层析柱层析法，膜过滤法，达到操作简单、减少成本投入的效果，同时提高了最终产品的品质并避免了废弃填料产生的环境污染等问题。
进一步地，所述有机溶剂为三氯甲烷、正己烷、正庚烷和正辛烷中的至少一种。
通过采用上述技术方案，在有机溶剂中，三氯甲烷、正己烷、正庚烷和正辛烷的实用性较强，在操作温度下稳定不易挥发，沸点适中，回收能耗小，便于完全去除；成本合适，不具备毒性。这几种有机溶剂可以混合使用，但会加大回收处理难度。
进一步地，所述步骤S4中，有机溶剂萃取的温度为50-90℃。
通过采用上述技术方案，在该温度范围下进行萃取，在合理控制能耗的基础上，由试验可知，可获得更快的萃取速度，且萃取效果更好。
进一步地，所述步骤S4中，浸膏的质量与有机溶剂的体积比为1:5-1:15。
通过采用上述技术方案，由试验可知，萃取更完全，萃取效果、效率更高。
进一步地，所述步骤S4中，有机溶剂分2-4次加入。
通过采用上述技术方案，由试验可知，萃取更完全，萃取效果、效率更高。
进一步地，每次加入有机溶剂后，萃取5-30min。
通过采用上述技术方案，由试验可知，萃取更完全，萃取效果更好。
进一步地，所述步骤S4中，萃取时持续搅拌。
通过采用上述技术方案，由试验可知，萃取更完全，萃取效果、效率更高。
进一步地，所述步骤S2中，大麻提取液浓缩至大麻二酚含量为1-5％后进行冬化处理。
通过采用上述技术方案，由试验可知，提高后续冬化除杂效果，最终进一步提高萃取效果。
综上所述，本申请具有以下有益效果：
1、本申请中优选采用预处理、浓缩、冬化、浸膏、脱羧和有机溶剂萃取，最后浓缩，完成大麻的除杂，达到操作简单、减少成本投入的效果，同时提高了最终产品的品质并避免了废弃填料产生的环境污染等问题。
2、本申请中优选采用三氯甲烷、正己烷、正庚烷和正辛烷的至少一种作为有机溶剂，实用性强，回收能耗小，成本适中。
3、本申请中优选萃取温度时间、有机溶剂用量，可获得更快的萃取速度，且萃取效果更好。
附图说明
图1是实施例22经过S3步骤后浸膏的液相色谱图；
图2是实施例22经过S5步骤后得到的大麻提取物的液相色谱图。
具体实施方式
以下结合附图对本申请作进一步详细说明。
实施例
实施例1：一种大麻除杂方法，包括以下步骤：
S1：预处理：将大麻花、叶收割，放入烘干机，在140℃的温度下进行烘干，烘干至含水量为5％；再送至粉碎机中进行粉碎，粉碎至60目及以上，得到原料粉；
称取60kg原料粉，将其以15kg/h的投料速度加入至逆流提取设备中，同时将480kg的95V/V乙醇水溶液以120L/h的进料速度持续进料至逆流提取设备，提取温度为25±5℃，提取60min，得到大麻提取液；
S2：将大麻提取液转移至真空低温浓缩设备，浓缩温度为50℃，浓缩至CBD含量为8％，加入95V/V乙醇水溶液调节至乙醇体积含量为60％，在60r/min的条件下搅拌5min；
再进行冬化处理：将添加了乙醇水溶液的大麻提取液放置于-50℃的温度静置24h后，再转移至板框式压滤设备进行过滤，除去杂质，得到过滤液；
将过滤液投入减压浓缩设备，在-0.09MPa的压强下浓缩至浸膏；
S3：将浸膏加热至140℃，直至无气泡产生停止加热，待用；
S4：向脱羧后的浸膏中加入有机溶剂，在25℃的温度下萃取40min，萃取结束后，转移至搅拌器中，加入浸膏质量50％的助滤剂，在20r/min的条件下搅拌10min，得到萃取液；
有机溶剂为二氯甲烷，浸膏质量与有机溶剂体积比为1:1；助滤剂为质量份数比为1:1的活性炭和硅藻土；
S5：将萃取液转移至减压浓缩设备，在-0.08MPa的压强下浓缩至除去有机溶剂，得到大麻 提取物。
实施例2：一种大麻除杂方法，与实施例1的区别在于：
S1中，烘干温度为150℃，烘干至含水量为1％；乙醇水溶液提取温度为35℃，提取时间为50min；
S2中，浓缩至CBD含量为10％，加入95V/V乙醇水溶液调节至乙醇体积含量为90％；冬化处理温度为-30℃，处理时间为28h，浓缩时压强为-0.08MPa；
S3中，加热温度为120℃；
S4中，有机溶剂为正壬烷，萃取温度为95℃，萃取时间为30min，浸膏质量与有机溶剂体积比为1：10。助滤剂使用量为浸膏质量的20％，助滤剂为硅藻土。
实施例3：一种大麻除杂方法，与实施例1的区别在于：
S1中，烘干温度为120℃，烘干至含水量为3％；乙醇水溶液提取温度为15℃，提取时间为75min；
S2中，浓缩至CBD含量为5％，加入95V/V乙醇水溶液调节至乙醇体积含量为85％；冬化处理温度为-60℃，处理时间为22h；
S3中，加热温度为150℃；
S4中，有机溶剂由质量份数比为1:1的三氯甲烷和正壬烷组成，萃取温度为45℃，萃取时间为40min，浸膏质量与有机溶剂体积比为1：20。助滤剂使用量为浸膏质量的10％，助滤剂为活性碳。
S5中，压强为-0.09MPa。
实施例4：一种大麻除杂方法，与实施例1的区别在于，有机溶剂为三氯甲烷。
实施例5：一种大麻除杂方法，与实施例1的区别在于，有机溶剂为正庚烷。
实施例6：一种大麻除杂方法，与实施例1的区别在于，有机溶剂由质量份数比为1:1:1的三氯甲烷、正己烷和正庚烷组成。
实施例7：一种大麻除杂方法，与实施例5的区别在于，萃取温度为50℃。
实施例8：一种大麻除杂方法，与实施例5的区别在于，萃取温度为70℃。
实施例9：一种大麻除杂方法，与实施例5的区别在于，萃取温度为90℃。
实施例10：一种大麻除杂方法，与实施例8的区别在于，浸膏质量与有机溶剂体积比为1：5。
实施例11：一种大麻除杂方法，与实施例8的区别在于，浸膏质量与有机溶剂体积比为1：10。
实施例12：一种大麻除杂方法，与实施例8的区别在于，浸膏质量与有机溶剂体积比为1：15。
实施例13：一种大麻除杂方法，与实施例12的区别在于，萃取次数为2次，将有机溶剂平均分为两份，每次添加一份且每次萃取时间为40min。
实施例14：一种大麻除杂方法，与实施例12的区别在于，萃取次数为3次，将有机溶剂平均分为三份，每次添加一份且每次萃取时间为40min。
实施例15：一种大麻除杂方法，与实施例12的区别在于，萃取次数为4次，将有机溶剂平均分为四份，每次添加一份且每次萃取时间为40min。
实施例16：一种大麻除杂方法，与实施例14的区别在于，每次萃取时间为5min。
实施例17：一种大麻除杂方法，与实施例14的区别在于，每次萃取时间为10min。
实施例18：一种大麻除杂方法，与实施例14的区别在于，每次萃取时间为30min。
实施例19：一种大麻除杂方法，与实施例17的区别在于，萃取时进行搅拌，搅拌速度为60r/min。
实施例20：一种大麻除杂方法，与实施例17的区别在于，萃取时进行搅拌，搅拌速度为30r/min。
实施例21：一种大麻除杂方法，与实施例19的区别在于，S2中，浓缩至CBD含量为1％。
实施例22：一种大麻除杂方法，与实施例19的区别在于，S2中，浓缩至CBD含量为5％。
上述实施例中，活性炭采购自江苏艾格尼丝环境科技有限公司，硅藻土采购自广州市昊兆化工有限公司。
对比例
对比例1：一种富含大麻二酚的火麻浸膏及其制备方法，将成熟的火麻花叶铺于一般的烘箱中，温度设为80℃，干热处理时间为3小时。然后用粉碎机将其研磨，取干燥的火麻花叶1.5千克，置于亚临界萃取装置的物料罐内，将溶剂罐中的亚临界状态的含40％乙醇的正丁烷注入物料罐内，于温度45℃，萃取压力0.6MPa下萃取45分钟。然后减压脱溶，将萃取物取出，重复萃取3次。将所得含浸膏的乙醇溶液加入一定量乙醇，使固液比达到1:7，然后置于-10℃的冰箱内进行冬化处理45分钟。然后利用-10℃，离心机进行离心处理20分钟。转速为4500转/分钟。所的上清液加入活性炭进行脱色处理，然后置于转速150转/分钟的摇床振荡25分钟。接着将上述混合物进行过滤操作，得过滤液。将滤液置于旋转蒸发瓶 中，在水浴温度50℃，转速50转/分钟的条件下进行旋蒸处理，得到大麻提取物。
对比例2：从工业大麻中提取二氢大麻酚(CBD)工艺，第1步，原料采用盛花期的花叶，花叶预先晒干或烤干，水份含量在10-15％之间，灰土含量在3％以下。把原料投入到烘烤设备内，温度控制在130-160℃之间(本对比例选用160℃)，时间控制在15-35分钟(本对比例选用20min)。
第2步，把烘干的花叶进行磨碎，达到5-10目之间。
第3步，把磨好的花叶装入浸泡器内进行浸泡，浸泡溶剂采用石油醚、正己烷或6#溶剂油。操作中为提高浸泡效果，可反复进行多次浸泡，浸泡温度不高于50℃(本对比例选用50℃)，浸泡时间每次不得低于1小时(本对比例选用1h)。浸泡后的混合溶液经过设备内的过滤网过滤后抽至浓缩器进行分离浓缩。
第4步，浓缩分离器，温度控制在90～120℃之间(本对比例选用100℃)。溶剂蒸发浓缩后剩余得到的固体、半固体膏状物即为富含CBD的浸膏。
对比例3：与实施例1的区别在于，将S1得到的大麻提取液进行浓缩，浓缩至CBD含量为8％，加入95V/V乙醇水溶液调节至乙醇体积含量为60％，在60r/min的条件下搅拌5min后，再进行冬化处理后先进行S3的脱羧，再投入减压浓缩设备，在-0.09MPa的压强下浓缩至浸膏。
对比例4：与实施例1的区别在于，与实施例1的区别在于，将S1得到的大麻提取液进行浓缩，浓缩至CBD含量为8％，加入95V/V乙醇水溶液调节至乙醇体积含量为60％，在60r/min的条件下搅拌5min后，先投入减压浓缩设备，在-0.09MPa的压强下浓缩至浸膏，再进行S3中的脱羧处理。
表征试验：
1、CBD含量及损耗率试验
试验对象：实施例1-22和对比例1-4，一共26组试验组。
试验方法：实施例1-22和对比例1-4从同一批原料粉中取料进行试验。在实施例1-22完成步骤S3后的浸膏取样进行CBD含量检测，并换算为80g中的CBD含量记录为萃取前浸膏的CBD含量，完成步骤S5后取样进行CBD含量检测，并换算为80g中的CBD含量记录为萃取后浸膏的CBD含量；计算CBD损耗率＝(CBD原始含量-萃取后浸膏的CBD含量)/CBD原始含量。对比例1-4将最后得到的大麻提取物或浸膏进行CBD含量检测。
CBD原始含量由实施例1的大麻提取液进行CBD含量检测得到，含量为40.2％。
CBD含量测量使用高效液相色谱仪，在柱温为30℃、流动相0.4ml/min、波长为 210nm的条件下进行检测，CBD标准品采购自长沙盈盛生物科技有限公司。
试验结果：实施例1-22、对比例1-3中CBD含量及损耗率试验结果记录如表1所示。
表1实施例1-22、对比例1-3中CBD含量及损耗率试验结果记录
Figure PCTCN2021131077-appb-000001
数据分析：如表1所示，与对比例相比，实施例在萃取后均表现出较高的CBD含量，且损耗率低。
对比实施例和对比例3-4的萃取前浸膏的CBD含量，说明萃取前的处理步骤参数以及处理步骤顺序对萃取前CBD的含量有影响，本实施例中采用的萃取前的步骤可有效提高萃取前浸膏的CBD含量，从而提高最终CBD的含量，提高大麻除杂效果。
与实施例1相比，实施例4-6限定了有机溶剂的组成，实施例7-9在实施例5的基础上进一步限定了萃取的温度，实施例10-12在实施例8的基础上进一步限定了有机溶剂的用量，均在其基础上进一步提高了CBD含量，且降低了损耗率。实施例13-15在实施例12的基础上增加了萃取次数，在实施例12的基础上大大提高了萃取后浸膏的CBD含量，说明萃取的参数对萃取效果和效率影响很大，实施例的优选参数可为萃取带来更好的萃取效果。
实施例16-18在实施例14的基础上限定了每次的萃取时间，可看出实施例16的效果差些，但到达10min每次时，效果就已经很好了，可以在节约能耗的基础上确保萃取效果。
实施例19-20在实施例17的基础上增加了搅拌，可以进一步提高萃取效果，可得到广泛的使用；且增加搅拌不易造成成本大幅上升，有利于控制处理成本。
另外，与过柱层析法和膜过滤除杂相比，可以大幅减少溶剂的使用量和资源的消耗。本申请中所采用的方法对比过柱层析法，可减少70％的溶剂使用量；对比膜过滤法，可降低设备成本，且溶剂使用量可减少30％。
2、除杂效果试验
试验对象：实施例22，一共1组试验样品。
试验方法：利用高效液相色谱仪对S3步骤后的浸膏，以及步骤S5中得到的大麻提取物，进行CBD成分检测。
试验结果：除杂效果试验如图1和图2所示。
数据分析：由图1和图2可知，经过步骤S3后，除杂效果很好，经过步骤S5后，除杂效果提升，且CBD损耗小。
本具体实施例仅仅是对本申请的解释，其并不是对本申请的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本申请的权利要求范围内都受到专利法的保护。

Claims (8)

  1. 一种大麻除杂方法，其特征在于，包括以下步骤：
    S1：预处理：将大麻花叶烘干、粉碎，得到原料粉；将原料粉用乙醇溶液进行提取，得到大麻提取液；
    S2：将大麻提取液浓缩之后，进行冬化处理，过滤后得到过滤液，将过滤液浓缩至浸膏；
    S3：将浸膏进行脱羧处理；
    S4：向脱羧后的浸膏中加入有机溶剂进行萃取，过滤后得到萃取液；
    S5：将萃取液浓缩除去有机溶剂后得到大麻提取物；
    所述有机溶剂为烷烃类或卤代烃中的至少一种。
  2. 根据权利要求1所述的一种大麻除杂方法，其特征在于，所述有机溶剂为三氯甲烷、正己烷、正庚烷和正辛烷中的至少一种。
  3. 根据权利要求1或2所述的一种大麻除杂方法，其特征在于，所述步骤S4中，有机溶剂萃取的温度为50-90℃。
  4. 根据权利要求1或2所述的一种大麻除杂方法，其特征在于，所述步骤S4中，浸膏的质量与有机溶剂的体积比为1:5-1:15。
  5. 根据权利要求1所述的一种大麻除杂方法，其特征在于，所述步骤S4中，有机溶剂分2-4次加入。
  6. 根据权利要求5所述的一种大麻除杂方法，其特征在于，每次加入有机溶剂后，萃取5-30min。
  7. 根据权利要求1所述的一种大麻除杂方法，其特征在于，所述步骤S4中，萃取时持续搅拌。
  8. 根据权利要求1所述的一种大麻除杂方法，其特征在于，所述步骤S2中，大麻提取液浓缩至大麻二酚含量为1-5％后进行冬化处理。
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