A method for preparing Ginseng radix volatile oil from steamed ginseng distillate

文档序号:1624214 发布日期:2020-01-14 浏览:18次 中文

阅读说明:本技术 一种以蒸参露为原料,制备人参挥发油的方法 (A method for preparing Ginseng radix volatile oil from steamed ginseng distillate ) 是由 曹志强 张宏桂 *** 马焕豪 李健豪 褚红涛 娄子恒 邹吉伟 苑冰冰 于 2019-10-11 设计创作,主要内容包括:本发明涉及人参挥发油的制备领域,即一种以蒸参露为原料,制备人参挥发油的方法。其步骤如下:(1)活性炭吸附挥发油:将人参蒸制加工成红参的过程中,所产生的“油、水”蒸气冷却成蒸参露并经活性炭过饱和吸附富集人参挥发油;(2)吸附后的活性炭脱水:沥水后自然阴干或甩干后阴干;(3)挥发油洗脱:用乙醚洗脱活性炭中人参挥发油;(4)分离制备:回收乙醚,得到人参挥发油成品。用上述加工工艺,可以大量富集蒸参露中人参挥发油,使鲜人参蒸制加工成红参过程中所产生的副产品蒸参露得以有效利用,并在最大限度上减少溶媒乙醚用量的条件下获得成品人参挥发油。(The invention relates to the field of preparation of ginseng volatile oil, in particular to a method for preparing ginseng volatile oil by taking steamed ginseng syrup as a raw material. The method comprises the following steps: (1) adsorbing volatile oil by activated carbon: during the process of steaming ginseng to prepare red ginseng, the generated oil and water vapor is cooled to prepare steamed ginseng distillate, and the steamed ginseng distillate is supersaturated by active carbon to adsorb and enrich ginseng volatile oil; (2) dehydrating the adsorbed activated carbon: naturally drying in the shade after draining or drying in the shade after spin-drying; (3) and (3) volatile oil elution: eluting Ginseng radix volatile oil with diethyl ether; (4) separation preparation: recovering diethyl ether to obtain Ginseng radix volatile oil product. The processing technology can enrich the ginseng volatile oil in the steamed ginseng juice in a large amount, so that the steamed ginseng juice which is a byproduct generated in the process of steaming and processing fresh ginseng into red ginseng can be effectively utilized, and the finished product of the ginseng volatile oil can be obtained under the condition of reducing the dosage of solvent diethyl ether to the maximum extent.)

1. A method for preparing ginseng volatile oil by taking steamed ginseng juice as a raw material is characterized by comprising the following steps:

(1) adsorbing volatile oil by activated carbon: during the process of steaming fresh ginseng to prepare red ginseng, the generated steam containing oil and water is cooled to prepare steamed ginseng distillate which is supersaturated and adsorbed by active carbon, thus achieving the purpose of enriching ginseng volatile oil;

(2) dehydrating the adsorbed activated carbon: naturally drying in the shade after draining or drying in the shade after spin-drying;

(3) and (3) volatile oil elution: eluting Ginseng radix volatile oil with diethyl ether;

(4) separation preparation: recovering diethyl ether to obtain Ginseng radix volatile oil product.

Technical Field

The invention relates to the field of preparation of ginseng volatile oil, in particular to a method for preparing ginseng volatile oil by taking ginseng steaming distillate which is a byproduct generated in the process of steaming fresh ginseng and processing the fresh ginseng into red ginseng as a raw material.

Background

Ginseng, the dry root and rhizome of Panax ginseng C.A. Meyer of Araliaceae, was listed as the top grade in Shen nong Ben Cao Jing, and has the effects of tranquilizing the mind, improving intelligence, reducing weight, prolonging life, and enjoying the reputation of Bai Cao Wang. Researches show that the main active substances in the ginseng comprise various components such as ginsenoside, ginseng polysaccharide, ginseng volatile oil, amino acid, polypeptide and the like. The saponin components in the ginseng are mainly divided into two types of tetracyclic triterpenes and pentacyclic triterpenes, the main pharmacological activities of the saponins are mostly applied to anti-tumor, anti-aging, fatigue relieving and the like, and at present, the researches on the field of extraction and preparation of the ginsenoside are more extensive and the technical application is more mature. The main chemical components of the ginseng volatile oil are sesquiterpene, aliphatic, aromatic and compounds represented by beta-limonene and panaxynol. The low-dose ginseng volatile oil has an exciting effect and a proper amount of tranquilizing effect, and besides, the synergistic effect of various components in the ginseng volatile oil can destroy the cell wall and cell membrane permeability of thalli, influence the energy metabolism of bacterial substances, and further have an inhibiting effect on staphylococcus aureus, actinomycetes, helicobacter pylori and the like, and common strains. Meanwhile, the ginseng volatile oil also has an anti-tumor effect, and pharmacological tests prove that the beta-myrcene and the panaxynol contained in the ginseng volatile oil have a strong inhibition effect on cancer cells, and are widely applied to various fields such as medicines, foods, cosmetics and the like. At present, the intensive research on the ginseng volatile oil is in a tense laboratory research stage, but because the content of the ginseng volatile oil is very low and the research and development costs are high, the effective action of the ginseng volatile oil does not make a prominent contribution to the 'big health' industry. At present, ginseng volatile oil is mainly extracted from ginseng roots, the content of the ginseng volatile oil in the ginseng roots is about 0.2 percent, and common extraction methods of the ginseng volatile oil comprise a steam distillation method, a solvent reflux method, a microwave method, a supercritical fluid extraction method and the like. Because the content of the volatile oil in the ginseng is relatively low, the cost and the final benefit required by taking the ginseng as the raw material for extracting the volatile oil are not proportional from the raw material or the production, so that the industrialized production is difficult to carry out.

As a main genuine production area of ginseng, Jilin province has tens of thousands of tons of fresh ginseng used as raw materials for processing red ginseng every year, nearly 80% of volatile oil is brought out along with water vapor (steamed ginseng juice) in the process of steaming and processing the fresh ginseng into the red ginseng, and the steamed ginseng juice generated in the part is generally discarded as waste as a byproduct in the process of processing the ginseng, so that not only is the environment polluted, but also great waste in resources is caused. According to the numerical calculation, more than 16000 kg of ginseng volatile oil is wasted every year (10000 tons multiplied by 1000 kg multiplied by 80 percent multiplied by 0.2 percent which is 16000 kg), and the loss of one item of the ginseng volatile oil every year is more than 32 hundred million yuan according to the current market price of the ginseng volatile oil which is calculated per kg of 20 ten thousand yuan.

At present, the ginseng volatile oil is extracted and prepared by using diethyl ether, petroleum ether, pentane, carbon tetrachloride and the like, wherein the diethyl ether and the petroleum ether have low boiling points and are well known ideal solvents. In the current extraction technology, solvent extraction is mainly used (the ratio of the ginseng steaming solution to the solvent is 1: 1). In view of safety, petroleum ether is usually selected in laboratories for preparing ginseng volatile oil. But the solvent used in the extraction process is extremely large and is not easy to recover, and the yield of the ginseng volatile oil is lower and is between 0.1 and 0.25 percent (patent application publication No.: CN 10/424817A). And the petroleum ether still has strong smell after being volatilized, so that the quality of the obtained ginseng volatile oil is poor and the ginseng volatile oil is difficult to meet the market requirement. The most preferable solvent for preparing the volatile oil of ginseng is diethyl ether, and considering the dosage and the production safety, a method of adsorbing the volatile oil of ginseng by a safe medium is preferably selected, a large amount of volatile oil of ginseng is firstly adsorbed, and then a small amount of diethyl ether is used for elution (the ratio of distilled ginseng juice to diethyl ether is 500-700: 1). High-quality ginseng volatile oil meeting the market requirement is obtained without reducing the yield, and a sufficient theoretical basis and technical support are provided for the industrial production of the ginseng volatile oil. Therefore, the technology can efficiently utilize the distilled ginseng juice which is a byproduct generated in the process of steaming and processing ginseng into red ginseng to carry out industrial preparation of the ginseng volatile oil, and good economic and social benefits are certainly brought.

Disclosure of Invention

The invention aims to provide a method for preparing ginseng volatile oil by taking ginseng distillate produced in the process of steaming fresh ginseng to prepare red ginseng as a raw material, aiming at the defects of the conventional preparation of the ginseng volatile oil. Firstly, condensing equipment is utilized to collect ginseng steaming dew, active carbon is used for supersaturated adsorption of ginseng volatile oil, and then a small amount of ether is used for elution (the ratio of the ginseng steaming dew to the ether is 500-700:1) to enrich and prepare the ginseng volatile oil, so that the purposes of changing waste into valuable, reducing cost and serving as 'big health' industry are achieved.

The technical solution of the invention is as follows: a method for preparing Ginseng radix volatile oil from distillate of Ginseng radix produced during steaming fresh Ginseng radix into Ginseng radix Rubri is provided. The method is characterized by comprising the following steps:

(1) adsorbing the ginseng volatile oil by using activated carbon: firstly, oil and water vapor generated in the process of steaming fresh ginseng to process the fresh ginseng into red ginseng is cooled into steamed ginseng juice, and the steamed ginseng juice is supersaturated and adsorbed by active carbon;

(2) dehydrating the adsorbed activated carbon: naturally drying in the shade after draining or drying in the shade after spin-drying;

(3) and (3) volatile oil elution: eluting Ginseng radix volatile oil with diethyl ether;

(4) separation preparation: recovering diethyl ether to obtain Ginseng radix volatile oil product.

The process is as follows:

1. the method for adsorbing and enriching the ginseng volatile oil by using the activated carbon comprises the following steps: connecting the air outlet pipe of the ginseng steaming tank with a condensing device, cooling oil and water vapor, inserting the ginseng steaming dew leading-out pipe into the bottom of a collecting barrel with an active carbon bag for reverse supersaturated adsorption, and stopping adsorption until the ginseng steaming dew flows out of the upper end of the collecting barrel and has the peculiar fragrance of the ginseng volatile oil.

2. The dehydration method of the adsorption saturated activated carbon comprises the following steps: draining, naturally drying in the shade or drying in the shade after spin-drying.

3. The volatile oil elution method comprises the following steps: loading the activated carbon which is supersaturated and adsorbed into a closed device, carrying out closed elution by using ether with a submerged volume at a low temperature (15-20 ℃), wherein the elution time of the ether is 10-30 min, and repeatedly eluting for 3-4 times.

4. The method for separating and preparing the ginseng volatile oil comprises the following steps: collecting the eluted oil-ether mixture, and recovering ether under reduced pressure. The temperature is controlled to be between 25 and 40 ℃, and the pressure is between 0.04 and 0.06 MPa.

The invention has the advantages that:

the method is characterized in that oil and water vapor generated in the process of steaming fresh ginseng to prepare red ginseng is cooled to prepare steamed ginseng distillate, the steamed ginseng distillate generated in the process of processing red ginseng is adsorbed and enriched by activated carbon supersaturated adsorption to serve as a processing raw material object, the ginseng volatile oil is adsorbed in a large amount by the activated carbon supersaturated adsorption technology, and then the ginseng volatile oil is eluted and separated by a small amount of solvent, so that the use amount of the solvent is greatly reduced, and the solvent is recovered to achieve the purpose of separating and preparing the ginseng volatile oil. The ginseng volatile oil is prepared by utilizing the ginseng steaming dew which is a byproduct generated in the process of steaming and processing fresh ginseng into red ginseng, so that the resource waste can be reduced, and the production cost can be reduced. The ginseng volatile oil product obtained by the invention can be used for research and production of medicines, health-care foods, foods and cosmetics.

The chemical component analysis test results of the ginseng volatile oil of the ginseng distillate obtained by different treatments in the same batch through GC-MS prove that the quantity and the relative content of the obtained components are almost the same as those of the ginseng distillate directly extracted by ether through the ginseng distillate absorbed by active carbon, the quality of the obtained volatile oil is not different, and the specific analysis results are shown in experimental examples 4-7.

Description of the drawings:

in order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the embodiments will be briefly described below, the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.

Fig. 1 is a process flow diagram provided in an embodiment of the present invention.

FIG. 2 is a total ion flow diagram of a ginseng volatile oil (some person in Jilin province, Ji' an City, joins the factory).

FIG. 3 is a total ion flow diagram of ginseng volatile oil (someone in Jingyu county, Jilin province attends the plant).

FIG. 4 is a total ion flow diagram of ginseng volatile oil (Jilin Ginseng research institute laboratory Ginseng processing).

FIG. 5 is a total ion flow diagram of ginseng volatile oil (Kangmei Xinkaihe ginseng processing plant husk activated carbon adsorbed oil "steamed ginseng distillate batch No. 20190925").

FIG. 6 is a total ion flow diagram of the ginseng volatile oil (ether directly extracted oil in Kangmei Xinkaihe ginseng processing plant "steamed ginseng distillate batch No. 20190925").

FIG. 7 is a total ion flow diagram of ginseng volatile oil (Cocos Nudifen Kokai No. 20190922) in the Cocos nucifera L.Don processing plant.

FIG. 8 is a total ion flow diagram of ginseng volatile oil (ether direct extract oil "steamed ginseng distillate batch No. 20190922" from Ji polymeric ginseng processing plant).

Detailed Description

In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.

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