CN111044626B - Preparation method of ginseng flower extract - Google Patents

Preparation method of ginseng flower extract Download PDF

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CN111044626B
CN111044626B CN201911172154.8A CN201911172154A CN111044626B CN 111044626 B CN111044626 B CN 111044626B CN 201911172154 A CN201911172154 A CN 201911172154A CN 111044626 B CN111044626 B CN 111044626B
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张语迟
刘春明
李赛男
赫岩
时东方
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Changchun Normal University
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Abstract

The invention provides a preparation method of a ginseng flower extract, belonging to the field of preparation of oil unsaponifiable matters. The method comprises processing dried flowers of Panax ginseng into powder, adding petroleum ether, extracting by reflux method, and pouring out petroleum ether solution after extraction; adding potassium hydroxide, n-hexane, methyl tert-butyl ether, acetonitrile and water into a petroleum ether solution, and stirring and heating; and standing after heating, and concentrating the uppermost petroleum ether layer under reduced pressure or normal pressure to obtain the ginseng flower extract. The detection of gas chromatography and mass spectrometry proves that the unsaponifiable matter sample in the ginseng flower oil obtained by the preparation method contains 6 chromatographic peaks, wherein the peak areas of 3 chromatographic peaks are large, the three chromatographic peaks are Stigmasterol, gamma-Sitosterol, Stigmast-7-en-3-ol, (3 beta, 5 alpha) -, and the three substances account for more than 93% of the total unsaponifiable matter by the normalization method.

Description

Preparation method of ginseng flower extract
Technical Field
The invention belongs to the field of preparation of oil unsaponifiable matters, and particularly relates to a preparation method of a ginseng flower extract.
Background
The ginseng flower is dried inflorescence of Panax ginseng C.A. Mey belonging to Araliaceae family. The wild species are distributed in northern Hebei, Liaoning, Jilin and Heilongjiang, the Liaoning and Jilin are cultivated widely, and the Beijing, Hebei and Shanxi are also cultivated by introduction. Collecting inflorescence in 6-7 months, and oven drying. Has the effects of invigorating qi, strengthening body constitution, and delaying aging. It is commonly used for dizziness, fatigue, chest distress and short breath. The flos Ginseng mainly contains saponin, chlorophyll, volatile oil and fatty oil. Modern medicine believes that ginseng flower has the effects of diminishing inflammation, inhibiting bacteria, resisting fatigue, resisting tumors and the like. Except saponin, volatile oil and fatty oil are important chemical components in ginseng flowers, and in order to detect the quality of oil, the quality of oil is often evaluated by taking 'unsaponifiable matters' as an index. The principle is as follows: after the oil and fat are saponified, some substances such as sterol, high molecular alcohol, hydrocarbon, pigment and fat-soluble vitamin are insoluble in water and soluble in organic solvent, and these substances are collectively called unsaponifiable matter. Conventionally, it is considered that the higher the content of unsaponifiable matter, the worse the quality of the oil and fat. However, recent researches prove that unsaponifiables in certain oils and fats also have quite strong biological activity, and the unsaponifiables in the preparation of the oils and fats or the extraction of the oils and fats can be used for developing foods, health-care foods, medicines and the like and can also be applied to the field of chemical engineering. When extracting oil from plant raw materials and preparing unsaponifiable matters in the oil by a traditional method, the oil is usually extracted from the raw materials firstly, an extraction solution is removed, potassium hydroxide and ethanol solution are added into the oil for heating and saponification, after saponification is finished, petroleum ether, diethyl ether and other solutions are used for extraction to obtain extracts of petroleum ether and diethyl ether layers, then the extracts are washed for multiple times by using alkali-containing ethanol and ethanol respectively, and the petroleum ether and the diethyl ether are volatilized to dryness to further obtain the unsaponifiable matters in the oil. The process needs 5 steps of extracting the grease from the raw material, preparing the grease, saponifying, extracting, washing and the like, the steps are relatively independent, and the operation is complicated. And the unsaponifiable matter needs to be washed for many times, thus increasing the preparation difficulty of the unsaponifiable matter.
The methods for preparing the grease unsaponifiable matters which are commonly adopted at present are mostly general methods or more complicated methods. The method for extracting unsaponifiable matters from the liquid shea butter, which is proposed by Huangxiancai and other Chinese patents (application number 201210181078.9), comprises the steps of ester exchange, molecular distillation, crystallization and the like, so that a high-purity unsaponifiable matter composition can be obtained, and the composition contains high content of triterpenoid alcohols and sterols; the antotun-bigri et al patent in china (application No. 201080047939.3) proposed a method for extracting unsaponifiable matter from renewable raw materials selected from the group consisting of oil-bearing fruits, oil-bearing seeds, etc., characterized in that it comprises the following steps: dehydrating, adding alcohol and catalyst, extracting, concentrating, saponifying, and extracting saponified material; j.le Ge Lang et al in Chinese patent (application No. 201280006964.6) propose the preparation method of total unsaponifiable matter of vegetable oil, which comprises the steps of firstly obtaining vegetable oil, saponifying with potassium carbonate ethanol solution, extracting with organic solution, recovering solvent, and stripping unsaponifiable matter with carrier gas. Zhandei et al, in Chinese patent (application No. 93118734.6), have proposed a preparation method of solanesol unsaponifiable matter, its main process is to regard mildew tobacco or broken miscellaneous tobacco powder as raw materials, add solvent and catalyst to carry on saponification, then carry on the process such as filtering, mixing, separating, hyperfiltration, concentration, etc., make solanesol unsaponifiable matter; in chinese patent application No. 201310739702.7, gazania zeoho et al, a two-stage column chromatography method for extracting squalene from deodorized distillate of vegetable oil was proposed, which was first saponified and comprised the following process steps: saponifying vegetable oil by common method, extracting and separating to obtain saponified substance, and separating squalene from unsaponifiable substance by column chromatography. The plum-tao et al chinese patent (application No. 201410828946.7) proposed a method for removing chlorophyll from microalgae by saponifying chlorophyll from green algae. The decoloration solution is sodium hydroxide ethanol solution, namely the method is a common saponification method. In summary, the methods described in the methods currently available are methods for saponifying vegetable oils by using common methods, or methods for saponifying vegetable oils by using transesterification and adding catalysts. In the method, the processes of extracting, saponifying and unsaponifiable matters of the vegetable oil are relatively independent, and the operation is complicated.
The ginseng flower oil contains saponified substances, unsaponifiable substances, chlorophyll, other impurities and the like, and the impurities can be extracted from the oil and still can not be saponified and still can be dissolved with the oil. In the conventional methods, when an unsaponifiable matter in an oil or fat is obtained, the oil or fat is often used as a material to be studied, and further subjected to treatments such as saponification and extraction. When plant raw materials are used as research materials, most of the plant raw materials need to be subjected to grease extraction, filtration, concentration, saponification, extraction and other treatments, and the traditional manual operation has multiple steps, is tedious and consumes long time. Especially, when the raw material contains chlorophyll, the treatment is more complicated.
Disclosure of Invention
The invention aims to provide a preparation method of a ginseng flower extract, which can remove saponified substances, chlorophyll and impurities in ginseng flowers so as to obtain unsaponifiable substances with high purity.
The invention provides a preparation method of a ginseng flower extract, which comprises the following steps and conditions:
the method comprises the following steps: processing dried flowers of Panax ginseng into powder, adding petroleum ether, extracting by reflux method, and pouring out petroleum ether solution after extraction;
step two: adding potassium hydroxide, n-hexane, methyl tert-butyl ether, acetonitrile and water into the petroleum ether solution obtained in the first step, and stirring and heating;
Step three: and standing after heating, dividing the solution into an upper layer, a middle layer and a lower layer, taking the uppermost layer, namely the petroleum ether layer, and concentrating under reduced pressure or normal pressure to obtain the ginseng flower extract.
Preferably, the extraction time of the first step is 0.5 to 2 hours.
Preferably, the volume V of petroleum ether in said first step1(ml): mass M of dried flower powder of Panax ginseng1(g) is (6-50): 1.
preferably, in the second step, the volume V of the virgin petroleum ether1(ml): volume V of n-hexane2(ml): volume V of methyl tert-butyl ether3(ml): volume V of acetonitrile4(ml): volume V of water5(ml): mass M of potassium hydroxide2(g) is 1: (0.5-2.0): (0.5-2.0): (1.0-2.0): (0.5-5.0): (0.02-0.05).
Preferably, the heating temperature in the second step is 90-300 ℃, the heating time is 0.5-2h, and the stirring speed is 100-300 rpm.
Preferably, the standing time in the third step is 60-600min
Preferably, the unsaponifiable matter contains Stigmasterol (Stigmasterol), gamma-Sitosterol (gamma-Sitosterol), Stigmast-7-en-3-ol, (3 beta, 5 alpha) -.
Principle of the invention
The invention relates to a preparation method of a ginseng flower extract, which is characterized in that petroleum ether is used for extracting grease in ginseng flower, the grease, chlorophyll and impurities are extracted together, after the extraction is finished and filtered, the concentration is not needed, n-hexane, methyl tert-butyl ether, acetonitrile, water and potassium hydroxide are directly added into an extracting solution for stirring and heating, so that a mixed solution of petroleum ether-n-hexane, methyl tert-butyl ether-acetonitrile-water-potassium hydroxide is formed, the mixed solution can be divided into an upper layer solution, a middle layer solution and a lower layer solution under the condition of no stirring, and an emulsion can be temporarily formed under the condition of stirring. Saponifying oil and chlorophyll in the emulsion, dissolving saponified product in methyl tert-butyl ether, acetonitrile and water, dissolving unsaponifiable product in petroleum ether, and dissolving impurities in n-hexane, methyl tert-butyl ether, acetonitrile and water. I.e. saponification and extraction are carried out simultaneously. And standing the mixture after the reaction is finished, and redistributing the mixed solution of petroleum ether-normal hexane, methyl tert-butyl ether-acetonitrile-water-potassium hydroxide into an upper layer solution, a middle layer solution and a lower layer solution. Wherein the high purity unsaponifiable matter is dissolved in the upper solution and the impurities are dissolved in the intermediate and lower solutions. Dissolving oil saponification substance and chlorophyll saponification substance in the middle and lower layer solutions, collecting the upper layer solution, and concentrating under reduced pressure. And then the synchronous operation of 'saponification and extraction of unsaponifiable matters' is completed, the rapid preparation from 'plant raw materials' to 'high-purity unsaponifiable matters' is realized, the impurities of the unsaponifiable matters of ginseng flower oil are reduced and the purity is improved by the extraction of two layers of solutions with different polarities, namely the high-purity unsaponifiable matters are obtained, the operation of repeatedly washing a petroleum ether layer by a traditional method is also avoided, the manual operation links are reduced, and the time and the reagents are saved.
The invention has the advantages of
The invention provides a preparation method of ginseng flower extract, which obtains a plant material extract in the form of paste, compared with the prior art, the method provided by the invention takes plant materials as research objects, directly adds reagents into an extracting solution after the first step of extraction, stirs and heats the extracting solution, completes saponification and multi-stage extraction by adopting a simpler method, and performs simultaneous saponification and extraction by using a mixed solution, the whole operation process is performed by one step, the manual operation links can also be reduced, the extraction steps are reduced, the extraction time is shortened, and the solution is effectively saved. Compared with the traditional method, the preparation rate of the unsaponifiable matters in the ginseng leaf oil is improved by about 50 percent, and the purity of the unsaponifiable matters is high.
The unsaponifiable matter mainly contains Stigmasterol (Stigmasterol), gamma-Sitosterol (gamma-Sitosterol), Stigmast-7-en-3-ol, (3 beta, 5 alpha) -, and the three substances account for more than 93 percent of the total unsaponifiable matter through a normalization method. The components are common chemical components in medicine, health food, chemistry and chemical industry, can be used for synthesizing steroid hormone, vitamin D3, progesterone and the like, can meet the development and utilization in the fields of medicine, food, chemistry and chemical industry, and have great application and development values.
Drawings
FIG. 1 is a gas chromatogram for detecting the ginseng flower extract (oil unsaponifiable matter) obtained in example 1 by a combination of gas chromatography and mass spectrometry.
FIG. 2 is a mass spectrum of Stigmasterol (Stigmasterol) which is a compound contained in the ginseng flower extract obtained in example 1;
FIG. 3 is a mass spectrum of a compound gamma-Sitosterol (gamma-Sitosterol) in the ginseng flower extract obtained in example 1;
FIG. 4 is a mass spectrum of Stigmast-7-en-3-ol, (3. beta., 5. alpha.) -compound in the ginseng flower extract obtained in example 1.
Detailed Description
The invention provides a preparation method of a ginseng flower extract, which comprises the following steps and conditions:
the method comprises the following steps: processing dried flowers of ginseng into powder, adding petroleum ether, extracting by a reflux method, wherein the extraction time is preferably 0.5-2h, and pouring out petroleum ether solution after the extraction is finished; volume V of said petroleum ether1(ml): mass M of dried flower powder of Panax ginseng1(g) is preferably (6-50): 1;
step two: adding potassium hydroxide, n-hexane, methyl tert-butyl ether, acetonitrile and water into the petroleum ether solution obtained in the first step, and stirring and heating; the heating temperature is preferably 90-300 ℃, the heating time is preferably 0.5-2h, and the stirring speed is preferably 100-30 0 rpm; volume V of the virgin petroleum ether1(ml): volume V of n-hexane2(ml): volume V of methyl tert-butyl ether3(ml): volume V of acetonitrile4(ml): volume V of water5(ml): mass M of potassium hydroxide2(g) is preferably 1: (0.5-2.0): (0.5-2.0): (1.0-2.0): (0.5-5.0): (0.02-0.05);
step three: and standing after heating, wherein the standing time is 60-600min, the solution is divided into an upper layer, a middle layer and a lower layer, the uppermost layer is a petroleum ether layer, and the petroleum ether layer is concentrated under reduced pressure or normal pressure to obtain the ginseng flower extract.
The preparation method provided by the invention obtains the extract rich in high-purity unsaponifiable matter of ginseng flower oil, and the obtained unsaponifiable matter extract of ginseng flower oil is detected by a gas chromatography-mass spectrometry combined method, wherein Stigmasterol (Stigmasterol), gamma-Sitosterol (gamma-Sitosterol), Stigmast-7-en-3-ol, (3 beta, 5 alpha) -is a common chemical component for medicine, health food, chemistry and chemical industry, can be used for synthesizing steroid hormone raw materials, can also be used as a production raw material of vitamin D3, can be used for biochemical research, preparation of progesterone, progesterone and the like.
The present invention is further illustrated by reference to the following specific examples, in which the starting materials are all commercially available.
Example 1
Processing dried ginseng flowers into powder, weighing 5g, adding 100mL of petroleum ether, extracting by a reflux method for 0.5 hour, filtering after extraction is finished, taking 91mL of petroleum ether extract, adding 2g of potassium hydroxide, 80mL of n-hexane, 80mL of methyl tert-butyl ether, 100mL of acetonitrile and 100mL of water into 91mL of petroleum ether solution, stirring and heating at the temperature: heating at 100 deg.C for 0.5 hr, stirring at 100rpm, standing for 60min after heating, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.
The relative amounts of Stigmasterol (Stigmasterol), γ -Sitosterol (γ -Sitosterol), Stigmast-7-en-3-ol, (3 β,5 α) -, were determined by the chromatographic peak areas using a combination of gas chromatography and mass spectrometry. The gas chromatograph-mass spectrometer comprises: model ITQ900 Thermo-Scientific in USA.
Mass spectrum parameters: a positive ion mode; emission current: 150 muA; electron energy: 70 eV; interface temperature: 300 ℃; ion source temperature: 230 ℃; detecting voltage: 1000V.
Chromatographic parameters: initial temperature of chromatography: 80 ℃; initialization time: 0.5 min; the heating rate is as follows: 15 deg/min; end temperature of chromatography: 250 ℃; end temperature residence time: and 15 min.
Sample introduction parameters: sample injector temperature: 280 ℃; sample introduction mode: constant current; flow rate: 1 ml/min; split mode, speed: 10 ml/min; chromatographic column DB-5ms, 30m 0.25mm 0.25 μm; carrier gas: and (e) He.
FIG. 1 is a gas chromatogram for measuring the ginseng flower extract (oil-and-fat unsaponifiable matter) obtained in example 1 by a combination of gas chromatography and mass spectrometry. Figure 1 shows that all chromatographic peaks elute essentially completely within 30 minutes and the resulting chromatographic peaks are completely separated. The sample chromatogram comprises 6 main chromatographic peaks, wherein the peak area of 3 chromatographic peaks is the largest, which shows that the content is higher, and the peak areas are Stigmasterol (Stigmasterol), gamma-Sitosterol (gamma-Sitosterol), Stigmast-7-en-3-ol, (3 beta, 5 alpha) -, and the content of the 3 compounds accounts for more than 93 percent of the total chemical components by utilizing a normalization method for calculation.
FIG. 2 is a mass spectrum of Stigmasterol (Stigmasterol) compound; FIG. 3 is a mass spectrum of a compound gamma-Sitosterol (gamma-Sitosterol); FIG. 4 is a mass spectrum of Stigmast-7-en-3-ol, (3 β,5 α) -; the mass spectrometry is applied to qualitatively identify chromatographic peaks in the total ion flow graph of the ginseng flower extract, and the result is as follows: chromatographic peak 1: 3,7,11, 15-tetramethylol-2-hexadecen-1-ol (matching degree 99%); chromatographic peak 2: stigmasterol (matching 99%); chromatographic peak 3: gamma-Sitosterol (matching degree 91%); chromatographic peak 4: stigmast-7-en-3-ol, (3 β,5 α) - (degree of match 99%); chromatographic peak 5: beta-Sitosterol (matching degree 90%); chromatographic peak 6: ergost-7-en-3-ol, (3. beta.) - (92% match).
Table 1 shows the peak area data of the ginseng flower extract obtained by gas chromatography and mass spectrometry.
TABLE 1 gas chromatography and Mass Spectrometry data for Panax ginseng flower extract
Figure BDA0002289006660000071
Example 2
Processing dried ginseng flowers into powder, weighing 5g, adding 150mL of petroleum ether, extracting by a reflux method for 1.0 hour, filtering after extraction is finished, adding 3.5g of potassium hydroxide, 150mL of n-hexane, 150mL of methyl tert-butyl ether, 160mL of acetonitrile and 200mL of water into 134mL of petroleum ether solution, stirring and heating at the temperature: heating at 150 deg.C for 1.0 hr, stirring at 150rpm, standing for 180min after heating, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.
Example 3
Processing dried ginseng flowers into powder, weighing 5g, adding 200mL of petroleum ether, extracting by a reflux method for 1.0 hour, filtering after extraction is finished, adding 4.0g of potassium hydroxide, 200mL of n-hexane, 200mL of methyl tert-butyl ether, 250mL of acetonitrile and 300mL of water into 184mL of petroleum ether solution, stirring and heating at the temperature: heating at 160 deg.C for 1.2 hr, stirring at 150rpm, standing for 300min after heating, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.
Example 4
Processing dried ginseng flowers into powder, weighing 5g, adding 150mL of petroleum ether, extracting by a reflux method for 1.5 hours, filtering after extraction is finished, adding 3.5g of potassium hydroxide, 200mL of n-hexane, 200mL of methyl tert-butyl ether, 200mL of acetonitrile and 250mL of water into 136mL of petroleum ether solution, stirring and heating at the temperature: heating at 140 deg.C for 1.5 hr, stirring at 200rpm, standing for 360min, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.
Example 5
Processing dried ginseng flowers into powder, weighing 5g, adding 100mL of petroleum ether, extracting by a reflux method for 1.5 hours, filtering after extraction is finished, adding 3.0g of potassium hydroxide, 100mL of n-hexane, 100mL of methyl tert-butyl ether, 120mL of acetonitrile and 150mL of water into 89mL of petroleum ether solution, stirring and heating at the temperature: heating at 150 deg.C for 1.5 hr, stirring at 250rpm, standing for 480min after heating, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.
Example 6
Processing dried ginseng flowers into powder, weighing 5g, adding 250mL of petroleum ether, extracting by a reflux method for 2.0 hours, filtering after extraction is finished, adding 12.5g of potassium hydroxide, 500mL of n-hexane, 500mL of methyl tert-butyl ether, 500mL of acetonitrile and 1250mL of water into 221mL of petroleum ether solution, stirring and heating at the temperature: heating at 300 deg.C for 2.0 hr, stirring at 300rpm, standing for 600min after heating, collecting petroleum ether layer, and concentrating under reduced pressure to obtain flos Ginseng extract.

Claims (5)

1. A preparation method of a ginseng flower extract is characterized by comprising the following steps and conditions:
the method comprises the following steps: processing dried flowers of Panax ginseng into powder, adding petroleum ether, extracting by reflux method, and pouring out petroleum ether solution after extraction;
step two: adding potassium hydroxide, n-hexane, methyl tert-butyl ether, acetonitrile and water into the petroleum ether solution obtained in the first step, and stirring and heating;
step three: standing after heating, dividing the solution into upper-middle-lower three layers, collecting the uppermost petroleum ether layer, and concentrating under reduced pressure or normal pressure to obtain flos Ginseng extract;
volume V of petroleum ether in the first step1: mass M of dried flower powder of Panax ginseng1In the volume of (6-50) ml: 1 g;
in the second step, the volume V of the virgin petroleum ether1: volume V of n-hexane2: volume V of methyl tert-butyl ether3: volume V of acetonitrile4: volume of waterV5: mass M of potassium hydroxide21 ml: (0.5-2.0) ml: (0.5-2.0) ml: (1.0-2.0) ml: (0.5-5.0) ml: (0.02-0.05) g;
the ginseng flower extract is an unsaponifiable matter.
2. The method for preparing ginseng flower extract according to claim 1, wherein the extraction time of the first step is 0.5-2 hours.
3. The method as claimed in claim 1, wherein the heating temperature in step two is 90-300 ℃, the heating time is 0.5-2h, and the stirring speed is 100-300 rpm.
4. The method for preparing ginseng flower extract according to claim 1, wherein the standing time in the third step is 60-600 min.
5. The method of claim 1, wherein the unsaponifiable matter comprises Stigmasterol, γ -Sitosterol, Stigmast-7-en-3-ol, (3 β,5 α) -.
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