CN105670798B - Extraction method of jujube kernel volatile oil - Google Patents

Extraction method of jujube kernel volatile oil Download PDF

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CN105670798B
CN105670798B CN201610118714.1A CN201610118714A CN105670798B CN 105670798 B CN105670798 B CN 105670798B CN 201610118714 A CN201610118714 A CN 201610118714A CN 105670798 B CN105670798 B CN 105670798B
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CN105670798A (en
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蒋卉
焦培培
于海峰
张娜
蔡雨晴
桂林康
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Tarim University
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/72—Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
    • A61K36/725—Ziziphus, e.g. jujube

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Abstract

The invention discloses a method for extracting jujube kernel volatile oil, which comprises the following steps: (1) pre-treating the jujube kernel raw material; (2) charging; (3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II; (4) carrying out static extraction; (5) dynamic primary extraction; (6) dynamic secondary extraction; (7) mixing the jujube kernel volatile oil obtained in the separation kettle I and the separation kettle II. The invention greatly improves the extraction efficiency of the jujube kernel volatile oil by adopting an extraction mode combining static extraction and dynamic extraction, and greatly improves the content of antioxidant compounds in the volatile oil by selecting a proper extracting agent.

Description

Extraction method of jujube kernel volatile oil
Technical Field
The invention belongs to the technical field of extraction of active ingredients of natural plants, and particularly relates to a method for extracting jujube kernel volatile oil.
Background
The semen Ziziphi Spinosae (Zizyphus jujube Mill) is dry mature kernel of Zizyphus in Zizyphus of Rhamnaceae, and mainly contains compounds such as jujube benevolence saponins, triterpenes, fatty oil, protein, sterols, phospholipids, etc. Modern pharmacological studies show that the jujube kernel has the effects of tonifying heart, tranquilizing, calming nerves, arresting sweating, tonifying liver, promoting the production of body fluid and the like, is used for treating symptoms such as dysphoria, insomnia, fright dreaminess, body deficiency, hyperhidrosis, body fluid deficiency, thirst and the like, and is a common sedative and hypnotic medicine. It is listed as the superior in Shen nong Ben Cao Jing (Shen nong's herbal Jing), and as the root system in Ben Cao gang mu (compendium of materia Medica). The medical books are originally seen in treatise on febrile diseases and famous in jujube kernel decoction, and have been in medicinal history for over 1700 years. The recent generation is recorded in the pharmacopoeia of the people's republic of China, a calendar edition. The volatile oil is one of the main active ingredients of the jujube kernel, and in recent years, the jujube kernel oil has been researched to have the same sedative-hypnotic effect as the jujube kernel gleditsia sinensis components, and is gradually an important research content of the jujube kernel.
The existing extraction method of jujube kernel volatile oil is roughly as follows: steam distillation, organic solvent extraction and supercritical fluid extraction. The former two methods have the problems of low yield, complicated process, unstable operation conditions and the like, and the supercritical CO2The fluid extraction method is a new extraction and separation technologyThe method is particularly suitable for extracting heat-sensitive substances, has the advantages of no heavy metal pollution, no solvent residue, convenient transportation, stable extraction conditions and the like, and can effectively improve the yield of target products by adding a proper amount of entrainer in the extraction process, but still has the problem of low extraction oil yield.
At present, the cultivation area of the Xinjiang jujube trees reaches 700 ten thousand mu, rich red jujube resources provide unique and advantageous conditions for the development and research of jujube kernels, and the processing of red jujubes has become an important link for the scale of the Xinjiang forest fruit planting industry and the income increase of farmers.
Disclosure of Invention
The invention aims to provide a method for extracting jujube kernel by using supercritical CO, aiming at the problems that the extraction yield of jujube kernel is low and raw materials cannot be effectively utilized2A method for extracting volatile oil from semen Ziziphi Spinosae by fluid extraction is provided.
A method for extracting jujube kernel volatile oil comprises the following steps:
(1) pre-treating the jujube kernel raw material: oven drying semen Ziziphi Spinosae, pulverizing, and sieving;
(2) charging: adding the pretreated semen Ziziphi Spinosae into supercritical CO2In an extraction kettle of a fluid extraction device;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to a preset pressure, and firstly, taking the solvent A as an entrainer to perform static extraction;
(5) dynamic primary extraction: CO regulation2The solvent A is taken as an entrainer to carry out dynamic primary extraction;
(6) dynamic secondary extraction: CO regulation2Finally adding a solvent B as an entrainer to perform dynamic secondary extraction;
(7) mixing the jujube kernel volatile oil obtained in the separation kettle I and the separation kettle II.
The extraction method of the jujube kernel volatile oil comprises the following steps of (1): the drying temperature of the jujube kernel is 45-65 ℃, the drying time is 15-25h, and the granularity of the crushed and sieved powder is 50-70 meshes.
The extraction method of the jujube kernel volatile oil comprises the following steps of (3): the extraction pressure of the extraction kettle is 20-35MPa, the extraction temperature is 35-50 ℃, the static extraction time is 0.5-1h, the dynamic primary extraction time is 1-2h, and the dynamic secondary extraction time is 2-3 h; the separation pressure of the separation kettle I is 8.0-9.0MPa, the separation temperature is 30-40 ℃, and the separation time is 1-3 h; the separation pressure of the separation kettle II is 4.9-5.8MPa, the separation temperature is 30-40 ℃, and the separation time is 0.5-2 h.
The extraction method of the jujube kernel volatile oil comprises the following steps (4) and (5): the solvent A is one of n-hexane, ethyl acetate and chloroform.
The extraction method of the jujube kernel volatile oil comprises the following steps of (6): the solvent B is n-butyl alcohol, tert-butyl methyl ether or a mixture of n-butyl alcohol and tert-butyl methyl ether.
The extraction method of the jujube kernel volatile oil comprises the following steps (5) and (6): the flow rate of CO2 is 1.0-1.5L/min.
The extraction method of the jujube kernel volatile oil has the advantage that the dosage of the solvent A is 20-30 wt% of the mass of the jujube kernel raw material.
In the extraction method of the jujube kernel volatile oil, the dosage of the solvent B is 50-100 wt% of the mass of the jujube kernel raw material.
The extraction method of the jujube kernel volatile oil also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material in the step (1); the alkali solution used for alkali soaking is a sodium carbonate solution with the mass concentration of 5-12 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 300-400mL, the alkali soaking time is 5-10h, and the filtering is carried out after the alkali soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 10-15 wt%, the dosage of the alkali solution of each 100g of jujube kernel powder is 200-300mL, the acid soaking time is 0.5-2h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 5-10 h.
The invention has the beneficial effects that: the method takes jujube kernels which are byproducts of red dates in the great forest of Xinjiang as raw materials, utilizes a supercritical CO2 extraction method to extract volatile oil from the jujube kernels, greatly improves the extraction efficiency of the volatile oil from the jujube kernels by adopting an extraction mode combining static extraction and dynamic secondary extraction, greatly improves the content of antioxidant compounds in the volatile oil by selecting a proper extracting agent, increases the medicinal value and the practical value of the volatile oil from the jujube kernels, improves the utilization rate of the jujube kernels, and increases the economic benefit of the jujube kernels.
Detailed Description
Example 1:
a method for extracting jujube kernel volatile oil comprises the following steps:
(1) pre-treating the jujube kernel raw material: oven drying semen Ziziphi Spinosae at 45 deg.C for 15 hr, pulverizing, and sieving to obtain powder with particle size of 50-70 mesh;
(2) charging: adding the pretreated semen Ziziphi Spinosae material and solvent A into supercritical CO2In an extraction kettle of a fluid extraction device; in the embodiment, the solvent A is n-hexane; the dosage of the solvent A is 20 wt% of the mass of the jujube kernel raw material;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
the extraction pressure of the extraction kettle is 20MPa, and the extraction temperature is 35 ℃; the separation pressure of the separation kettle I is 8.0MPa, and the separation temperature is 30 ℃; the separation pressure of the separation kettle II is 4.9MPa, and the separation temperature is 30 ℃;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to the set pressure in the step (3), and firstly, taking the solvent A as an entrainer to perform static extraction for 0.5 h;
(5) dynamic primary extraction: CO regulation2The flow rate of the solvent A is 1.0L/min, and then the solvent A is taken as an entrainer to carry out dynamic primary extraction for 1 h;
(6) dynamic secondary extraction: CO regulation2The flow rate of the extraction kettle is 1.0L/min, and finally, a solvent B is added into the extraction kettle by an entrainer pump to be used as an entrainer for dynamic secondary extraction, wherein the dynamic secondary extraction time is 2 hours; the solvent B is n-butyl alcohol, and the dosage of the solvent B is 50 wt% of the mass of the jujube kernel raw material;
(7) separating in separation kettle I for 1 hr and separation kettle II for 0.5 hr, and mixing the volatile oils obtained in separation kettle I and separation kettle II.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 32.02%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 14.23 units/mg.
Example 2:
a method for extracting jujube kernel volatile oil comprises the following steps:
(1) pre-treating the jujube kernel raw material: oven drying semen Ziziphi Spinosae at 65 deg.C for 25 hr, pulverizing, and sieving to obtain powder with particle size of 50-70 mesh;
(2) charging: adding the pretreated semen Ziziphi Spinosae material and solvent A into supercritical CO2In an extraction kettle of a fluid extraction device; in this example, solvent a is ethyl acetate; the dosage of the solvent A is 30 wt% of the mass of the jujube kernel raw material;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
the extraction pressure of the extraction kettle is 35MPa, and the extraction temperature is 50 ℃; the separation pressure of the separation kettle I is 9.0MPa, and the separation temperature is 40 ℃; the separation pressure of the separation kettle II is 5.8MPa, and the separation temperature is 40 ℃;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to the set pressure in the step (3), and firstly, taking the solvent A as an entrainer to perform static extraction for 1 h;
(5) dynamic primary extraction: CO regulation2The flow rate of the solvent A is 1.5L/min, and then the solvent A is taken as an entrainer to carry out dynamic primary extraction for 2 hours;
(6) dynamic secondary extraction: CO regulation2The flow rate of the extraction kettle is 1.5L/min, and finally, a solvent B is added into the extraction kettle by an entrainer pump to be used as an entrainer for dynamic secondary extraction, wherein the dynamic secondary extraction time is 3 hours; the solvent B is tert-butyl methyl ether, and the using amount of the solvent B is 100 wt% of the mass of the jujube kernel raw material;
(7) separating in separation kettle I for 3h and separation kettle II for 2h, and mixing the volatile oil obtained in separation kettle I and separation kettle II.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 34.72%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 15.46 units/mg.
Example 3:
a method for extracting jujube kernel volatile oil comprises the following steps:
(1) pre-treating the jujube kernel raw material: oven drying the semen Ziziphi Spinosae at 50 deg.C for 17 hr, pulverizing, and sieving to obtain powder with particle size of 50-70 mesh;
(2) charging: adding the pretreated semen Ziziphi Spinosae material and solvent A into supercritical CO2In an extraction kettle of a fluid extraction device; in the embodiment, the solvent A is one of trichloromethane; the dosage of the solvent A is 22 wt% of the mass of the jujube kernel raw material;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
the extraction pressure of the extraction kettle is 30MPa, and the extraction temperature is 40 ℃; the separation pressure of the separation kettle I is 8.5MPa, and the separation temperature is 35 ℃; the separation pressure of the separation kettle II is 5.0MPa, and the separation temperature is 35 ℃;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to the set pressure in the step (3), and firstly, taking the solvent A as an entrainer to perform static extraction for 0.8 h;
(5) dynamic primary extraction: CO regulation2The flow rate of the solvent A is 1.2L/min, and then the solvent A is taken as an entrainer to carry out dynamic primary extraction, wherein the dynamic primary extraction time is 1.5 h;
(6) dynamic secondary extraction: CO regulation2The flow rate of the extraction kettle is 1.3L/min, and finally, a solvent B is added into the extraction kettle by an entrainer pump to be used as an entrainer for dynamic secondary extraction, wherein the dynamic secondary extraction time is 2.5 h; the solvent B is a mixture of n-butyl alcohol and tert-butyl methyl ether, and the using amount of the solvent B is 60 wt% of the mass of the jujube kernel raw material;
(7) separating in separation kettle I for 2h and separation kettle II for 1h, and mixing the volatile oil obtained in separation kettle I and separation kettle II.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 33.13%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 16.23 units/mg.
Example 4:
a method for extracting jujube kernel volatile oil comprises the following steps:
(1) pre-treating the jujube kernel raw material: oven drying semen Ziziphi Spinosae at 60 deg.C for 23 hr, pulverizing, and sieving to obtain powder with particle size of 50-70 mesh;
(2) charging: adding the pretreated semen Ziziphi Spinosae material and solvent A into supercritical CO2In an extraction kettle of a fluid extraction device; in this example, solvent a is ethyl acetate; the dosage of the solvent A is 25 wt% of the mass of the jujube kernel raw material;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
the extraction pressure of the extraction kettle is 32MPa, and the extraction temperature is 45 ℃; the separation pressure of the separation kettle I is 8.3MPa, and the separation temperature is 33 ℃; the separation pressure of the separation kettle II is 5.4MPa, and the separation temperature is 36 ℃;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to the set pressure in the step (3), and firstly, taking the solvent A as an entrainer to perform static extraction for 0.7 h;
(5) dynamic primary extraction: CO regulation2The flow rate of the solvent A is 1.4L/min, and then the solvent A is taken as an entrainer to carry out dynamic primary extraction, wherein the dynamic primary extraction time is 1.5 h;
(6) dynamic secondary extraction: CO regulation2The flow rate of the extraction kettle is 1.4L/min, and finally, a solvent B is added into the extraction kettle by an entrainer pump to be used as an entrainer for dynamic secondary extraction, wherein the dynamic secondary extraction time is 2.2 h; the solvent B is a mixture of n-butyl and tert-butyl methyl ether, the volume ratio of n-butyl to tert-butyl methyl ether is 1:3, and the amount of the solvent B is 80 wt% of the mass of the jujube kernel raw material;
(7) separating in separation kettle I for 2.5 hr and separation kettle II for 1.5 hr, and mixing the volatile oils obtained in separation kettle I and separation kettle II.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 35.58%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 17.24 units/mg.
Example 5:
this example differs from example 1 in that: the step (1) also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material; the alkaline solution used for alkaline soaking is a sodium carbonate solution with the mass concentration of 5 wt%, the dosage of the alkaline solution per 100g of jujube kernel powder is 300mL, the alkaline soaking time is 5h, and the filtering is carried out after the alkaline soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 10 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 200mL, the acid soaking time is 0.5h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 5 h.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 37.36%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 14.89 units/mg.
Example 6:
this example differs from example 2 in that: the step (1) also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material; the alkaline solution used for alkaline soaking is a sodium carbonate solution with the mass concentration of 12 wt%, the dosage of the alkaline solution per 100g of jujube kernel powder is 400mL, the alkaline soaking time is 10h, and the filtering is carried out after the alkaline soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 15 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 300mL, the acid soaking time is 2h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 10 h.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 38.89%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 15.87 units/mg.
Example 7:
this example differs from example 3 in that: the step (1) also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material; the alkaline solution used for alkaline soaking is a sodium carbonate solution with the mass concentration of 10 wt%, the dosage of the alkaline solution per 100g of jujube kernel powder is 350mL, the alkaline soaking time is 8h, and the filtering is carried out after the alkaline soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 12 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 250mL, the acid soaking time is 1h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 8 h.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 37.75%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 16.99 units/mg.
Example 8:
this example differs from example 4 in that: the step (1) also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material; the alkaline solution used for alkaline soaking is a sodium carbonate solution with the mass concentration of 7 wt%, the dosage of the alkaline solution per 100g of jujube kernel powder is 360mL, the alkaline soaking time is 9h, and the filtering is carried out after the alkaline soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 11 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 300mL, the acid soaking time is 2h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 6 h.
The mass of the jujube kernel volatile oil is finally obtained by weighing, the yield of the obtained jujube kernel volatile oil is 39.26%, and the total antioxidant capacity of the volatile oil tested by a T-AOC kit method is 17.59 units/mg.
From examples 5 to 8 it can be seen that: after alkali soaking, acid soaking and buffer solution soaking are sequentially carried out, the yield of the jujube kernel volatile oil is greatly improved, and the total antioxidant capacity of the obtained volatile oil is not greatly changed. However, if the sequence of alkali soaking, acid soaking and buffer solution soaking is changed, the yield of the jujube kernel volatile oil is reduced by more than 30 percent when the jujube kernel volatile oil is not soaked, and the total antioxidant capacity of the volatile oil is reduced by more than 10 percent when the jujube kernel volatile oil is not soaked.
The above examples are provided for clarity of illustration only and are not intended to limit the invention to the particular embodiments described. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any obvious variations or modifications which come within the spirit and scope of the invention are desired to be protected by the following claims.

Claims (1)

1. The extraction method of the jujube kernel volatile oil is characterized by comprising the following steps:
(1) pre-treating the jujube kernel raw material: oven drying semen Ziziphi Spinosae, pulverizing, and sieving; the drying temperature of the jujube kernels is 60 ℃, the drying time is 23 hours, and the granularity of the crushed and sieved powder is 50-70 meshes; the step (1) also comprises the steps of sequentially carrying out alkali soaking, acid soaking, buffer solution soaking and air drying on the crushed and sieved jujube kernel raw material; the alkaline solution used for alkaline soaking is a sodium carbonate solution with the mass concentration of 7 wt%, the dosage of the alkaline solution per 100g of jujube kernel powder is 360mL, the alkaline soaking time is 9h, and the filtering is carried out after the alkaline soaking; the acid solution used for acid soaking is hydrochloric acid with the mass concentration of 11 wt%, the dosage of the alkali solution per 100g of jujube kernel powder is 300mL, the acid soaking time is 2h, and the filtering is carried out after the acid soaking; the buffer solution used for soaking is phosphoric acid buffer solution with pH 7.2, and the soaking time of the buffer solution is 6 h;
(2) charging: adding the pretreated semen Ziziphi Spinosae material and solvent A into supercritical CO2In an extraction kettle of a fluid extraction device; in this example, solvent a is ethyl acetate; the dosage of the solvent A is 25 wt% of the mass of the jujube kernel raw material;
(3) setting the temperature and pressure of the extraction kettle, the separation kettle I and the separation kettle II;
the extraction pressure of the extraction kettle is 32MPa, and the extraction temperature is 45 ℃; the separation pressure of the separation kettle I is 8.3MPa, and the separation temperature is 33 ℃; the separation pressure of the separation kettle II is 5.4MPa, and the separation temperature is 36 ℃;
(4) static extraction: introducing a certain amount of CO2Raising the pressure in the extraction kettle to the set pressure in the step (3), and firstly, taking the solvent A as an entrainer to perform static extraction for 0.7 h;
(5) dynamic primary extraction: CO regulation2The flow rate of the solvent A is 1.4L/min, and then the solvent A is taken as an entrainer to carry out dynamic primary extraction, wherein the dynamic primary extraction time is 1.5 h;
(6) dynamic secondary extraction: CO regulation2The flow rate of the extraction kettle is 1.4L/min, and finally, a solvent B is added into the extraction kettle by an entrainer pump to be used as an entrainer for dynamic secondary extraction, wherein the dynamic secondary extraction time is 2.2 h; the solvent B is a mixture of n-butyl and tert-butyl methyl ether, the volume ratio of n-butyl to tert-butyl methyl ether is 1:3, and the amount of the solvent B is 80 wt% of the mass of the jujube kernel raw material;
(7) separating in separation kettle I for 2.5 hr and separation kettle II for 1.5 hr, and mixing the volatile oils obtained in separation kettle I and separation kettle II.
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CN106433956A (en) * 2016-11-28 2017-02-22 无限极（中国）有限公司 Method for extracting volatile oil
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