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CN115028613B - Method for extracting lutein ester and quercitin from marigold flowers - Google Patents

Method for extracting lutein ester and quercitin from marigold flowers Download PDF

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CN115028613B
CN115028613B CN202210741682.6A CN202210741682A CN115028613B CN 115028613 B CN115028613 B CN 115028613B CN 202210741682 A CN202210741682 A CN 202210741682A CN 115028613 B CN115028613 B CN 115028613B
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quercitin
extracting
lutein ester
lutein
marigold
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CN115028613A (en
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刘温来
赵辰光
田芸
李勇
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Shandong Tianyin Biotechnology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40—Separation, e.g. from natural material; Purification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00—Derivatives 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
    • C07C403/24—Derivatives 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A method for extracting lutein ester and quercitin from marigold flowers belongs to the technical field of plant active ingredient extraction. The method is characterized by comprising the following steps of: 1) Subcritical extracting flos Tagetis Erectae by using a mixed solvent of dimethyl ether and butane, wherein the mass ratio of flos Tagetis Erectae to the mixed solution is 1:3-12, and the mass ratio of dimethyl ether to butane in the mixed solvent is 1:2-8, so as to obtain an extracting solution; 2) Concentrating the extracting solution into a mixture containing lutein ester and quercitin, wherein the solid content in the mixture is 92% -96%; 3) And (3) extracting and separating the mixture obtained in the step (2) by using a methanol solvent to obtain two products of the quercitin and the lutein ester. The invention solves the problem of high harmful residue of lutein ester and quercitin in the prior product, and solves the problem that the lutein ester active substance is easy to be destroyed.

Description

Method for extracting lutein ester and quercitin from marigold flowers
Technical Field
A method for extracting lutein ester and quercitin from marigold flowers belongs to the technical field of plant active ingredient extraction.
Background
Quercetin (QG) belongs to flavonol compounds, is one of main components of Tagetes erecta belonging to Compositae, and has certain antioxidant capacity. The quercitin is a natural antioxidant extracted from marigold and has the advantages of safety, high efficiency and the like.
At present, a stepwise extraction method is mainly adopted for the extraction method of lutein and flavone. Chinese patent 201811188771.2 discloses an industrialized preparation method of lutein and marigold flavone, which adopts a mixed solvent of petroleum ether and acetone for extraction, wherein the separation mode adopted in the patent is that water is added for separation, the operation is complex, high-purity quercetin marigold can not be obtained through separation, and only marigold flavone mixture can be obtained.
Chinese patent CN110746331a discloses an industrial method for extracting lutein and quercitin from marigold flower particles, comprising the following steps: 1) Extracting the marigold flower particles by using an acetone solution with the volume fraction of 90-99% to obtain an extracting solution; 2) Concentrating the extract until the solid content is 60-95%, and extracting the concentrate with low-polarity solvent to obtain the quercus marigold and lutein products. The invention can extract lutein and quercitin simultaneously. However, the lutein and the quercitin are extracted by using 90% -99% of acetone solution, the boiling point of the extraction solvent acetone is high, the toxicity of the solvent is high, the loss of the lutein ester as an active ingredient in the process of extracting and purifying the product is high, and the acetone residue in the product is high.
Chinese patent 201811188771.2 discloses an industrialized preparation method of lutein and marigold flavone, which is mainly improved in that lutein extraction solvent petroleum ether and flavone extraction solvent are mixed, marigold flower particles are extracted, and after extraction is completed, strong polar solvent is added into the flavone extraction solvent, so that separation of lutein and marigold flavone is further promoted. The invention can improve the extraction efficiency, and the invention adopts the mixed solvent of petroleum ether and acetone, and also has the phenomenon that the solvent residue in the product is difficult to remove.
There is still a lack of a safe method for extracting lutein and querceting marigold.
Disclosure of Invention
The invention aims to solve the technical problems that: overcomes the defects of the prior art and provides a method for extracting lutein ester and quercetin from flos Tagetis Erectae without harmful residues.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for extracting lutein ester and quercitin from marigold flowers is characterized by comprising the following steps of:
1) Subcritical extracting flos Tagetis Erectae by using a mixed solvent of dimethyl ether and butane, wherein the mass ratio of flos Tagetis Erectae to the mixed solution is 1:3-12, and the mass ratio of dimethyl ether to butane in the mixed solvent is 1:2-8, so as to obtain an extracting solution;
2) Concentrating the extracting solution into a mixture containing lutein ester and quercitin, wherein the solid content in the mixture is 92% -96%;
3) And (3) extracting and separating the mixture obtained in the step (2) by using a methanol solvent to obtain two products of the quercitin and the lutein ester.
The invention mainly provides a novel mixed solvent capable of simultaneously extracting lutein ester and quercitin from marigold flowers, and harmful residues can be avoided under the conditions of high-efficiency and high-yield extraction by utilizing the mixed solvent, and meanwhile, active substances can be prevented from being damaged in the extraction process. The mixed solvent can be easily and thoroughly separated from the extract after subcritical extraction. The extract is extracted and separated by methanol solvent, and two products of high-purity quercitin and lutein ester are obtained.
Preferably, the method for extracting lutein ester and quercitin from marigold flowers comprises the following steps of 1) mixing the marigold flowers with a mixed solution: 5 to 8. The preferable ratio of flos Tagetis Erectae to the mixed solution can reduce the solvent consumption as much as possible while ensuring the yield of the two products.
More preferably, the method for extracting lutein ester and quercetin from flos Tagetis Erectae comprises the following steps of 1) mixing flos Tagetis Erectae with a mixed solution: 5.3 to 6.1. The maximum yield of the invention can be achieved in the case of a mixed solvent in which the ratio of the optimal marigold flower to the mixed solution is further suitable.
Preferably, the mass ratio of dimethyl ether to butane in the mixed solvent in the step 1) is 1:4 to 6. The mixed solvent is obtained by mixing dimethyl ether and butane in a subcritical state, and the preferable proportion can better adapt to the extraction requirement of the invention, and can extract lutein ester and quercitin simultaneously with high yield.
More preferably, the mass ratio of dimethyl ether to butane in the mixed solvent in the step 1) is 1:4.7 to 5.2. The most preferable mixed solvent ratio can reach the maximum extraction yield of the invention.
Preferably, the subcritical extraction temperature in the step 1) is 25-50 ℃, the extraction times are 3-6, and the extraction time of each time is 15-60 min. The optimized subcritical extraction process can thoroughly extract lutein ester and quercitin in marigold flowers, and ensures high yield of the invention.
Preferably, the method for extracting lutein ester and quercetin from flos Tagetis Erectae comprises the step 3) of extracting 75-85% of methanol in methanol solvent. The preferred methanol solvent can better extract and separate the extract, thereby ensuring the high purity of the extracted product.
Preferably, the mass ratio of the mixture in the step 3) to the methanol solvent is 1:5 to 10. The preferred mass ratio of the mixture to the methanol solvent enables a more thorough separation of the two products.
Preferably, the method for extracting lutein ester and quercetin from flos Tagetis Erectae comprises the step 3) of extracting and separating at 65-90deg.C. The two products are easier to separate under the extraction solvent of the invention at the preferential extraction temperature, and the separation is ensured to be thorough.
Preferably, the method for extracting lutein ester and quercetin from flos Tagetis Erectae comprises the step 2) wherein the solid content of the mixture is 94% -95%. The preferable solid content can ensure that the extraction is carried out smoothly and the purity of the lutein ester product at the lower layer after the extraction is ensured.
Compared with the prior art, the method for extracting lutein ester and quercitin from marigold has the following beneficial effects: the invention uses subcritical method to extract lutein ester and quercetin two functional active components from flos Tagetis Erectae. The invention mainly provides a novel mixed solvent capable of simultaneously extracting lutein ester and quercitin from marigold flowers, and harmful residues can be avoided under the conditions of high-efficiency and high-yield extraction by utilizing the mixed solvent, and meanwhile, active substances can be prevented from being damaged in the extraction process. The mixed solvent can be easily and thoroughly separated from the extract after subcritical extraction. The extract is extracted and separated by methanol solvent, and two products of high-purity quercitin and lutein ester are obtained. The invention mainly aims at solving the problems of high harmful residues of lutein ester and quercitin in the existing product and the problem that the lutein ester active substance is easily damaged in the existing extraction method.
Detailed Description
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise, and the terms "comprising" and "having" and any variation thereof are intended to cover a non-exclusive inclusion, e.g., a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements explicitly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other.
The invention will be further described with reference to specific examples, of which example 1 is the best practice.
The marigold flowers related in the embodiment are from Shandong Tianyin biotechnology limited company, can be directly purchased in the market, and are dried and granulated by the conventional process to obtain the marigold particles.
Example 1
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 116kg of 5 mixed liquid, extraction 4 times at 40 ℃ for 30min each.
2) Concentrating the extractive solution under reduced pressure, mixing 4 times of concentrated extracts, wherein the concentration of the extract is 95%, and the concentration is 6.03kg.
3) Adding 42kg of methanol with the volume ratio of 80% into the concentrated solution, heating and stirring at 70 ℃ for 60min, slowly cooling to 50 ℃ and standing for 6 hours, wherein the lower layer of oil layer is lutein ester, and the upper layer is quercitin.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 2
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:5.2 mixed liquor 106kg, extracted 4 times at 45 ℃ for 40min each time.
2) Concentrating the extractive solution under reduced pressure, mixing 4 times of concentrated extracts, wherein the concentration of the extract is 95%, and the concentration is 6.01kg.
3) Adding 48.08kg of 82% methanol into the concentrated solution, heating at 80deg.C, stirring for 55min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin marigold.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 3
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:4.7 mixed liquor 122kg, extracted 4 times at 35 ℃ for 25min each time.
2) The extracts were concentrated each time under reduced pressure, and the extracts from 4 times of concentration were combined to give an extract concentration of 94% and a concentrate weight of 6.01kg.
3) Adding 78% methanol 36.06kg, heating at 75deg.C, stirring for 58min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 4
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:4 mixed liquor 100kg, extracted 5 times at 30 ℃ for 20min each time.
2) Concentrating the extractive solution under reduced pressure, mixing 5 times of concentrated extracts, wherein the concentration of the extract is 93%, and the concentration of the concentrate is 5.95kg.
3) Adding 35.7kg of 80% methanol into the concentrated solution, heating and stirring at 85deg.C for 52min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin marigold.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 5
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:6 mixed liquor 160kg, extracted 4 times at 40 ℃ for 50min each time.
2) Concentrating the extractive solution under reduced pressure, mixing 4 times of concentrated extracts, wherein the concentration of the extract is 95.5%, and the concentration is 6.03kg.
3) Adding 54.27kg of 80% methanol into the concentrated solution, heating and stirring at 68deg.C for 60min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin Tagetin.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 6
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:2 mixed liquor 60kg, extraction 6 times at 50 ℃ for 15min each.
2) The extract was concentrated under reduced pressure each time, and the 6 concentrated extracts were combined to give an extract concentration of 96% and a concentrate weight of 5.89kg.
3) Adding 58.9kg of methanol with volume ratio of 85%, heating and stirring at 65deg.C for 65min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin Tagetin.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 7
1) 20kg of marigold flower particles with the lutein content of 28g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the compressed mass ratio of: butane = 1:8 mixed liquor 240kg, extraction 3 times at 25 ℃ for 60min each.
2) The extract was concentrated under reduced pressure each time, and the extracts of 3 times of concentration were combined, the concentration of the extract was 92%, and the concentrate mass was 6.04kg.
3) Adding 30.2kg of 75% methanol into the concentrated solution, heating at 90deg.C, stirring for 50min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin marigold.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 8
1) 25kg of marigold flower particles with the lutein content of 26g/kg are taken and transferred into a subcritical extraction kettle, and dimethyl ether with the mass ratio of compression is added: butane = 1:4 mixed liquid 100kg, extraction 4 times at 40 ℃ for 30min each time;
2) The extracts were concentrated each time under reduced pressure, and the extracts from 4 times of concentration were combined to give an extract concentration of 94% and a concentrate weight of 7.4kg.
3) 70kg of 84% methanol is added into the concentrated solution, the mixture is heated and stirred for 60min at 70 ℃, the temperature is slowly reduced to 50 ℃ and the mixture is kept stand for 6 hours, the lower layer oil layer is lutein ester, and the upper layer is quercitin.
Discharging and continuously concentrating the lower lutein ester layer to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Example 9
1) Taking 10kg of marigold flower particles with the lutein content of 30g/kg, transferring into a subcritical extraction kettle, and adding dimethyl ether with the compressed mass ratio: butane = 1:3 mixed liquid 100kg, extraction 4 times at 45 ℃ for 30min each time;
2) The extracts were concentrated each time under reduced pressure, and the extracts from 4 times of concentration were combined to give an extract concentration of 94% and a concentrate weight of 7.4kg.
3) Adding 95% methanol 75kg, heating at 70deg.C, stirring for 60min, slowly cooling to 50deg.C, standing for 6 hr, wherein the lower oil layer is lutein ester, and the upper layer is quercetin.
Discharging the lutein ester for the next time and continuously concentrating to obtain a lutein ester product; the upper layer of the quercitin layer is continuously cooled to 30 ℃ and kept stand for 120min, and the quercitin is obtained after filtration and drying.
Quercetin detection conditions:
mobile phase A is 2% phosphoric acid solution, phase B is ethylene wax, and analysis is carried out by gradient elution (gradient elution conditions are shown in Table 1); the elution flow rate is 1mL/min; column temperature: 40 ℃; chromatographic column CORTECS C18 column (4.6mm.times.50mm, particle size 2.7 μm); ultraviolet detector wavelength: 260nm; sample injection amount: 2. Mu.L.
TABLE 1
Time min Flow rate, mL/min A，％ B，％
Initial initiation 1 88.0 12.0
5.0 1 88.0 12.0
5.5 1 10.0 90.0
7.5 1 10.0 90.0
8.0 1 88.0 12.0
9.0 1 88.0 12.0
The lutein ester detection method comprises the following steps:
and detecting the content of lutein ester under 445nm by adopting an ultraviolet spectrophotometry.
Lutein esters and quercetin lutein detection results are shown in table 2.
TABLE 2
The embodiment shows that the lutein ester and the champs-elyseed skin tagetes obtained by the method have higher yield and purity.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (2)

1. A method for extracting lutein ester and quercitin from marigold flowers, which is characterized by comprising the following steps:
1) Subcritical extracting the marigold flowers by using a mixed solvent of dimethyl ether and butane, wherein the extracting temperature is 25-50 ℃, the extracting times are 3-6 times, the extracting time of each time is 15-60 min, the mass ratio of the marigold flowers to the mixed solution is 1:5.3-6.1, and the mass ratio of the dimethyl ether to the butane in the mixed solvent is 1:4.7-5.2, so as to obtain an extracting solution;
2) Concentrating the extracting solution into a mixture containing lutein ester and quercitin, wherein the solid content in the mixture is 92% -96%;
3) Extracting and separating the mixture obtained in the step 2) at 65-90 ℃ by using a methanol solvent to obtain two products of quercitin and lutein ester, wherein the volume fraction of methanol in the methanol solvent is 75-85%, and the mass ratio of the mixture to the methanol solvent is 1:5 to 10.
2. The method for extracting lutein ester and quercetin from flos Tagetis Erectae according to claim 1, wherein the method comprises the following steps:
the solid content in the mixture in the step 2) is 94-95%.
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