CN108948785A - The extracting method of pigment in a kind of Cordyceps militaris - Google Patents

The extracting method of pigment in a kind of Cordyceps militaris Download PDF

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Publication number
CN108948785A
CN108948785A CN201811199945.5A CN201811199945A CN108948785A CN 108948785 A CN108948785 A CN 108948785A CN 201811199945 A CN201811199945 A CN 201811199945A CN 108948785 A CN108948785 A CN 108948785A
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China
Prior art keywords
cordyceps militaris
pigment
fruiting bodies
extracting method
added
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CN201811199945.5A
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Inventor
詹怀敬
杨军
颜迟
贾俊杰
詹怀利
周兰
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Anhui Xiangkang Bioengineering Co Ltd
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Anhui Xiangkang Bioengineering Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
    • C07C403/24Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096Purification; Precipitation; Filtration
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)

Abstract

The invention belongs to Cordyceps militaris effective component extractive technique fields, and in particular to the extracting method of pigment in a kind of Cordyceps militaris.It is of the present invention extract Cordyceps militaris in pigment method, in the prior art using ethyl alcohol as Extraction solvent on the basis of, further addition sarcosine as assisted extraction, effectively increase the recovery rate of pigment in Cordyceps militaris;The method of the present invention for extracting pigment in Cordyceps militaris, further uses the supplementary mode of ultrasonic disperse during the extraction process, further improves the recovery rate of pigment;More preferably, in the method for the invention, before extracting, by way of impregnating fruiting bodies of cordyceps militaris in polyglycol solution, the dissolution of pigment has been effectively facilitated, it helps improve the recovery rate of pigment.

Description

The extracting method of pigment in a kind of Cordyceps militaris
Technical field
The invention belongs to Cordyceps militaris effective component extractive technique fields, and in particular to the extraction side of pigment in a kind of Cordyceps militaris Method.
Background technique
Cordyceps militaris (Cordycepsmilitaris (L.) Link) also known as northern Chinese caterpillar Fungus, are under the jurisdiction of Eumycota (Eumycota), Ascomycota (Ascomycota), Ascomycotina (Ascomycotinia), excrement shell Gammaproteobacteria (Sordariomycetes), meat seat bacterium subclass (Hypocreomycetidae), Hypocreales (Hypocreales), cordyceps sinensis section (Cordycipitaceae), the type sepecies of Cordyceps (Cordyceps).Cordyceps militaris usually has similar life with cordyceps sinensis Object active constituent mainly includes cordycepin, cordycepic acid, Cordyceps sinensis polysaccharide, ergosterol, amino acid, nucleosides material etc., Cordyceps militaris The effect of it is also similar to cordyceps sinensis, be the good substitute of cordyceps sinensis.Cordyceps militaris is a kind of natural resources, shows the world Property distribution, but quantity is seldom, and majority is cultivated by artificial plantation.In recent years, chemical component and pharmacology of the mankind to artificial aweto Activity conducts extensive research, the results showed that, the chemical component of artificial aweto, pharmacological effect and natural cs are essentially identical, Wherein Cordyceps sinensis polysaccharide, cordycepin content be also more than natural cs.Largely modern pharmacological studies have shown that Cordyceps militaris not only has There is special nutritive value, and has apparent medical value.
The appearance of Cordyceps militaris show it is orange-yellow, the reason is that because itself contained by uranidin caused by.It was found that pupa Cordyceps sinensis pigment is a Carotenoids, since in the carotenoid that finds so far, mostly fat-soluble class is recklessly Radish element, is not easy to be absorbed by the body and some meet that photo-thermal are unstable, and Cordyceps militaris uranidin is then that one kind for finding so far is rare The water-soluble carotenoid seen.
Carotenoid is the major class pigment in the world's ecosystems, very extensive in natural distribution, carotenoid As the precursor of vitamin A, help to prevent and eradicate vitamine A deficiency, meanwhile, carotenoid also has a variety of biologies Activity, such as anti-inflammatory, anticancer, oxidation resistant effect.Carotenoid not only can increase body as important nutrient source Disease-prevention health, immune function, and medical industry, food, in terms of it is widely used.Cordyceps militaris uranidin is as class Hu One kind of radish element theoretically has stronger potential physiological activity compared with traditional carotenoid.
At present in the extracting method of Cordyceps militaris uranidin, there are mainly two types of: one is first use Flavonoids by Macroporous Adsorption Resin pair Crude extract carries out rough segmentation, then is isolated and purified using normal-phase silica gel column chromatography;Another kind is through Primary organic solvents such as ethyl alcohol After purification, it is carried out using preparation liquid phase isolated.But the former has that complex steps, yield are not high, and due to Purification on normal-phase silica gel load capacity is small, causes to recycle more difficult;And the latter's method but also there is process costs height, can not achieve The problem of large-scale production;Therefore, a kind of method for developing fermentation and the extraction of carotenoid suitable for Cordyceps militaris, has Positive meaning.
Summary of the invention
For this purpose, technical problem to be solved by the present invention lies in a kind of extracting method of pigment in Cordyceps militaris is provided, with solution The certainly not high problem of pigment extraction efficiency in Cordyceps militaris in the prior art.
In order to solve the above technical problems, in a kind of Cordyceps militaris of the present invention pigment extracting method, including walk as follows It is rapid:
(1) it is dry to take fruiting bodies of cordyceps militaris, and crushes, it is spare;
(2) ethanol solution is added into gained fruiting bodies of cordyceps militaris powder to mix, and sarcosine is added and extracts.
Preferably, the additional amount of the sarcosine accounts for the 2-5wt% of the fruiting bodies of cordyceps militaris amount.
The solid-liquid ratio of the fruiting bodies of cordyceps militaris and the ethanol solution is 1:20-30, and the unit of the solid-liquid ratio is g/ The relationship of mL.
Preferably, the ethanol solution is the ethanol water of mass ratio 60-80%.
Preferably, the sarcosine is extracted that treated 30-60min is added ethyl alcohol is added.
Preferably, the ethanol extraction step carries out under ultrasound condition.
Preferably, the power of the ultrasonic step is 100-150W.
It preferably, further include that the fruiting bodies of cordyceps militaris is placed in polyglycol solution to soak in the step (1) The step of stain processing.
Preferably, the solid-liquid ratio of the fruiting bodies of cordyceps militaris and the polyethylene glycol is 1:10-20.
Specifically, the polyglycol solution is the polyethylene glycol 400 aqueous solution of mass concentration 40-60wt%.
The method of the present invention for extracting pigment in Cordyceps militaris, in the prior art using ethyl alcohol as the basis of Extraction solvent On, sarcosine is further added as assisted extraction, effectively increases the recovery rate of pigment in Cordyceps militaris;Extraction of the present invention The method of pigment in Cordyceps militaris further uses the supplementary mode of ultrasonic disperse during the extraction process, further improves pigment Recovery rate;More preferably, in the method for the invention, before extracting, by by fruiting bodies of cordyceps militaris in polyethylene glycol The mode impregnated in solution has effectively facilitated the dissolution of pigment, it helps improves the recovery rate of pigment.
Specific embodiment
Embodiment 1
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 20L that mass concentration is 80% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, and to mixed It closes and the mixing of 20g sarcosine is added in liquid, the extraction 2h of carotenoid is carried out under room temperature, collect extract.
Embodiment 2
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 30L that mass concentration is 60% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, and to mixed It closes and the mixing of 50g sarcosine is added in liquid, the extraction 2h of carotenoid is carried out under room temperature, collect extract.
Embodiment 3
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, and to mixed It closes and the mixing of 35g sarcosine is added in liquid, the extraction 2h of carotenoid is carried out under room temperature, collect extract.
Embodiment 4
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 30min, 35g sarcosine is added into the Extraction solvent and mixes, continues 90min is extracted, extract is collected.
Embodiment 5
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 60min, 35g sarcosine is added into the Extraction solvent and mixes, continues 60min is extracted, extract is collected.
Embodiment 6
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, extract is collected.
Embodiment 7
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, entire extraction process is carried out under ultrasound condition, and the power for controlling the ultrasonic step is 100W, is received Collect extract.
Embodiment 8
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, entire extraction process is carried out under ultrasound condition, and the power for controlling the ultrasonic step is 150W, is received Collect extract.
Embodiment 9
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, entire extraction process is carried out under ultrasound condition, and the power for controlling the ultrasonic step is 125W, is received Collect extract.
Embodiment 10
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) it takes fruiting bodies of cordyceps militaris to be placed in the polyethylene glycol 400 aqueous solution of mass concentration 40wt% and carries out impregnation 2h, the solid-liquid ratio for controlling the fruiting bodies of cordyceps militaris and the polyethylene glycol is 1:20g/mL;Poly- second two is removed after impregnation Alcoholic solution, and by treated, the fruiting bodies of cordyceps militaris is dried to constant temperature in 50 DEG C, the Cordyceps militaris after taking above-mentioned drying Fructification 1kg, and through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, entire extraction process is carried out under ultrasound condition, and the power for controlling the ultrasonic step is 125W, is received Collect extract.
Embodiment 11
The extracting method of pigment, includes the following steps: in Cordyceps militaris described in the present embodiment
(1) it takes fruiting bodies of cordyceps militaris to be placed in the polyethylene glycol 400 aqueous solution of mass concentration 60wt% and carries out impregnation 2h, the solid-liquid ratio for controlling the fruiting bodies of cordyceps militaris and the polyethylene glycol is 1:10g/mL;Poly- second two is removed after impregnation Alcoholic solution, and by treated, the fruiting bodies of cordyceps militaris is dried to constant temperature in 50 DEG C, the Cordyceps militaris after taking above-mentioned drying Fructification 1kg, and through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction for carrying out carotenoid;And after extracting 45min, 35g sarcosine is added into the Extraction solvent and mixes, continues 75min is extracted, entire extraction process is carried out under ultrasound condition, and the power for controlling the ultrasonic step is 125W, is received Collect extract.
Comparative example 1
The extracting method of pigment uses the usual manner of the prior art in Cordyceps militaris described in this comparative example, that is, includes following step It is rapid:
(1) fruiting bodies of cordyceps militaris is taken to be dried in 50 DEG C to constant temperature, the fruiting bodies of cordyceps militaris 1kg after taking above-mentioned drying, And through conventional crushing, fruiting bodies of cordyceps militaris powder is made, it is spare;
(2) the ethanol solution 25L that mass concentration is 70% is added into above-mentioned fruiting bodies of cordyceps militaris powder to mix, in room temperature The lower extraction 2h for carrying out carotenoid, collects extract.
Experimental example
The extracting solution collected in above-described embodiment 1-11 and comparative example 1 is taken to carry out the detection of cordyceps sinensis pigment content, tool respectively Body is measured using ultraviolet spectrophotometer method conventional in the prior art, the maximum of carotenoid known in the state of the art Absorbing wavelength is 448nm, measures the light absorption value of solution at that wavelength, and calculate each extinction for extracting sample according to standard curve The content concn of the corresponding carotenoid of value, and the content of carotenoid in the extracting solution is calculated relative to Cordyceps militaris with this The extraction efficiency of carotenoid content, is recorded in the following table 1 in fructification.
1 Cordyceps militaris pigment recovery rate result of table
The method that can be seen that pigment in extraction Cordyceps militaris of the present invention from upper table data, in the prior art with second On the basis of alcohol is as Extraction solvent, sarcosine is further added as assisted extraction, effectively increases pigment in Cordyceps militaris Recovery rate;The method of the present invention for extracting pigment in Cordyceps militaris, further uses the auxiliary of ultrasonic disperse during the extraction process Mode further improves the recovery rate of pigment;More preferably, in the method for the invention, before extracting, by by pupa The mode that cordyceps militaris sporocarp impregnates in polyglycol solution has effectively facilitated the dissolution of pigment, it helps improve pigment Recovery rate.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or It changes still within the protection scope of the invention.

Claims (10)

1. the extracting method of pigment in a kind of Cordyceps militaris, which comprises the steps of:
(1) it is dry to take fruiting bodies of cordyceps militaris, and crushes, it is spare;
(2) ethanol solution is added into gained fruiting bodies of cordyceps militaris powder to mix, and sarcosine is added and extracts.
2. the extracting method of pigment in Cordyceps militaris according to claim 1, which is characterized in that the additional amount of the sarcosine Account for the 2-5wt% of the fruiting bodies of cordyceps militaris amount.
3. the extracting method of pigment in Cordyceps militaris according to claim 1 or 2, which is characterized in that Cordyceps militaris is real The solid-liquid ratio of body and the ethanol solution is 1:20-30, and the unit of the solid-liquid ratio is the relationship of g/mL.
4. the extracting method of pigment in Cordyceps militaris according to claim 1-3, which is characterized in that the ethyl alcohol is molten Liquid is the ethanol water of mass ratio 60-80%.
5. the extracting method of pigment in Cordyceps militaris according to claim 1-4, which is characterized in that the sarcosine It is to extract that treated 30-60min is added ethyl alcohol is added.
6. the extracting method of pigment in Cordyceps militaris according to claim 1-5, which is characterized in that the ethyl alcohol mentions Step is taken to carry out under ultrasound condition.
7. the extracting method of pigment in Cordyceps militaris according to claim 6, which is characterized in that the power of the ultrasonic step For 100-150W.
8. the extracting method of pigment in Cordyceps militaris according to claim 1-7, which is characterized in that the step (1) in, further include the steps that for the fruiting bodies of cordyceps militaris being placed in progress impregnation in polyglycol solution.
9. the extracting method of pigment in Cordyceps militaris according to claim 8, which is characterized in that the fruiting bodies of cordyceps militaris with The solid-liquid ratio of the polyethylene glycol is 1:10-20g/mL.
10. the extracting method of pigment in Cordyceps militaris according to claim 8 or claim 9, which is characterized in that the polyethylene glycol is molten Liquid is the polyethylene glycol 400 aqueous solution of mass concentration 40-60wt%.
CN201811199945.5A 2018-10-16 2018-10-16 The extracting method of pigment in a kind of Cordyceps militaris Pending CN108948785A (en)

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CN109998983A (en) * 2019-05-14 2019-07-12 安发(福建)生物科技有限公司 A kind of moist lipstick of the extract containing Cordyceps militaris and preparation method thereof
CN116970290A (en) * 2023-06-28 2023-10-31 安发(福建)生物科技有限公司 Cordyceps militaris pigment extract and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109998983A (en) * 2019-05-14 2019-07-12 安发(福建)生物科技有限公司 A kind of moist lipstick of the extract containing Cordyceps militaris and preparation method thereof
CN116970290A (en) * 2023-06-28 2023-10-31 安发(福建)生物科技有限公司 Cordyceps militaris pigment extract and preparation method and application thereof

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