CN113750071B - Preparation method of wolfberry polysaccharide-wolfberry seed oil soft capsule - Google Patents
Preparation method of wolfberry polysaccharide-wolfberry seed oil soft capsule Download PDFInfo
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- CN113750071B CN113750071B CN202110973356.3A CN202110973356A CN113750071B CN 113750071 B CN113750071 B CN 113750071B CN 202110973356 A CN202110973356 A CN 202110973356A CN 113750071 B CN113750071 B CN 113750071B
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- polysaccharide
- wolfberry
- lycium barbarum
- seed oil
- soft capsule
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- 235000015459 Lycium barbarum Nutrition 0.000 title claims abstract description 253
- 235000015468 Lycium chinense Nutrition 0.000 title claims abstract description 195
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- 239000007901 soft capsule Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 150000004676 glycans Chemical class 0.000 claims abstract description 156
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- 239000008518 lycium barbarum polysaccharide Substances 0.000 claims abstract description 96
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims abstract description 54
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 39
- 238000006467 substitution reaction Methods 0.000 claims abstract description 25
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims abstract description 24
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
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- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 6
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- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
- A61K36/815—Lycium (desert-thorn)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
- A61K9/4825—Proteins, e.g. gelatin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4841—Filling excipients; Inactive ingredients
- A61K9/4858—Organic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
- A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
- A61P37/04—Immunostimulants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Health & Medical Sciences (AREA)
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- Pharmacology & Pharmacy (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Immunology (AREA)
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Abstract
The invention provides a preparation method and application of wolfberry polysaccharide, and belongs to the technical field of food processing. The preparation method comprises the specific steps of extraction of lycium barbarum polysaccharide, molecular modification of lycium barbarum polysaccharide, extraction of lycium barbarum seed oil and preparation of lycium barbarum polysaccharide-lycium barbarum seed oil soft capsules. The invention has the beneficial effects that: the sorbitan monooleate is added to completely fuse the lycium barbarum polysaccharide and the lycium barbarum seed oil, so that the sedimentation of emulsified liquid can be prevented, layering and flocculation of the lycium barbarum polysaccharide-lycium barbarum seed oil are prevented, the added acetyl group enables the quantity of the hydroxyl groups in the lycium barbarum polysaccharide to be replaced by acetyl to be about 8-10%, and proper acetyl is added into the lycium barbarum polysaccharide, so that the emulsifying property of the lycium barbarum polysaccharide is improved; certain carboxymethyl is added to the wolfberry polysaccharide to make the hydroxyl substituted by carboxymethyl with the substitution degree of about 5-10%, so that the capability of the wolfberry polysaccharide-wolfberry seed oil in immunoregulation, antioxidation and other characteristics is improved.
Description
Technical Field
The invention relates to the technical field of food processing, in particular to a preparation method of a wolfberry polysaccharide-wolfberry seed oil soft capsule.
Background
The medlar is a dried mature fruit of the Ningxia medlar of the perennial shrub plant of the Solanaceae, has sweet taste and smooth property, and has the effects of tonifying essence and improving eyesight, nourishing liver and kidney, nourishing yin and moistening lung, and tonifying deficiency and tonifying essence. Medlar is also widely used as a dietary supplement in addition to pharmaceutical use. The fructus Lycii contains phenylpropyl esters, flavones, polyphenols, polysaccharides, etc., wherein more than 50% of fructus Lycii polysaccharide. Has the biological functions of regulating immunity, resisting oxidation and aging, protecting liver, reducing blood pressure, reducing blood sugar, regulating blood lipid, enhancing cell activity, etc. The medlar seed oil is called as vascular scavenger, and the content of unsaturated fatty acid, linolenic acid and oleic acid is up to more than 85 percent. The medlar polysaccharide and medlar seed oil can be prepared into capsules; in the preparation of the traditional wolfberry polysaccharide-seed oil capsule, the prepared product has the advantages of general quality, higher production cost and certain irrational property in the technical process.
Because the wolfberry polysaccharide molecules have hydrophilicity and are oleophobic molecules, the wolfberry polysaccharide molecules cannot be well combined with wolfberry seed oil, and after the wolfberry polysaccharide-wolfberry seed oil products of the prior art indexes are placed for a period of time, the phenomenon of polysaccharide flocculation precipitation can occur, so that the product quality is affected.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a wolfberry polysaccharide-wolfberry seed oil soft capsule, which can effectively solve the problems in the background technology.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4 preparation of Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule
S1, extracting wolfberry polysaccharide, which comprises the following steps:
s11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing and sieving to obtain Chinese wolfberry powder;
s12, mixing the medlar powder obtained in the step S11 according to a feed liquid ratio of 1:7 to 1:5, adding purified water in proportion, performing microwave treatment at normal temperature, performing ultrasonic treatment, filtering, and collecting filtrate;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane, wherein the treatment time is 100-500 min, the inlet and outlet pressure is 2.6/2-2.8/1.9 Bar, the treatment temperature is 38-54 ℃, filtering and concentrating, then passing through an ultrafiltration membrane, filtering and concentrating again, the treatment time is 25-225 min, the inlet and outlet pressure is 2-35/2-34.5Bar, the treatment temperature is 15-39 ℃, and collecting concentrated solution;
S14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide.
The medlar polysaccharide extracted in the step S1 is prepared into 50% medlar polysaccharide water solution with the viscosity of 300 mPa.s-400 mPa.s.
S2, modifying wolfberry polysaccharide molecules, which comprises the following steps:
s21, adding 10 parts of medlar polysaccharide into 100 parts of formamide organic solvent according to mass fraction, adding 2 parts of pyridine, stirring and mixing thoroughly, and adding 10 parts of acetic anhydride;
s22, stirring the material obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 10 parts of the lycium barbarum polysaccharide obtained in the step S22, adding 150 parts of formamide solvent, stirring for 2 hours, adding 5 parts of 20% sodium hydroxide aqueous solution, simultaneously adding 3 parts of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 15-24 hours by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the lycium barbarum polysaccharide containing acetyl and carboxymethyl;
the substitution degree of acetyl in the wolfberry polysaccharide is 8-10%, and the substitution degree of carboxymethyl is 5-10%.
The medlar polysaccharide with acetyl groups obtained in the step S22 is prepared into 50 percent medlar polysaccharide water solution with the mass fraction, the viscosity is 450 to 500 mPa.s,
The medlar polysaccharide with acetyl and carboxymethyl obtained in the step S23 is prepared into 50% medlar polysaccharide aqueous solution with the mass fraction, and the viscosity is 400 mPas-450 mPas.
S3, extracting medlar seed oil, which comprises the following steps:
s31, rinsing and sun-drying the wolfberry residues after the wolfberry polysaccharide is extracted, controlling the water content to be less than or equal to 5%, crushing the wolfberry residues by a ten-thousand-level crusher, and crushing the wolfberry seeds to 30 meshes.
S32, supercritical extraction: liquid CO with flow rate of 550L/min is pumped by a high-pressure pump at 28MPa 2 Pumping into extraction kettle, mixing with fructus Lycii seed, and extracting under supercritical state at 33deg.C.
S33, separation: the temperature of the separation kettle is raised to 40-45 ℃ and the pressure is controlled to 10-12MPa, so that the carbon dioxide is changed from a liquid state to a gaseous state, and is separated from the medlar seed oil and recycled.
S34, filtering: the separated medlar seed oil is filtered by a rectifying kettle, and impurities in the medlar seed oil are filtered out by adopting 300-mesh filter cloth and stored in a storage tank temporarily.
S4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, which comprises the following steps:
s41, preparing the lycium barbarum polysaccharide obtained in the step S2 into a lycium barbarum polysaccharide aqueous solution with the concentration of 35-65%;
s42, weighing the wolfberry polysaccharide obtained in the step S41 and the wolfberry seed oil obtained in the step S3 according to a certain proportion, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device;
S43, adding sorbitan monooleate accounting for 3% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
s45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
The mass fraction ratio of the wolfberry polysaccharide aqueous solution to the wolfberry seed oil in the step S4b is 1:0.8 to 1.2.
The soft capsule content obtained in the step S43 has a viscosity of 550 mPas to 600 mPas.
Preferably, the screening in step S11 is a 40 mesh screen.
Preferably, in the step S12, the feed liquid ratio is 1: and 6, performing microwave treatment to obtain microwave power of 300w and treatment time of 10mi < n >.
Preferably, in the step S13, the treatment time is 100mi n and the treatment temperature is 38 ℃.
Preferably, the ceramic film in the step S12 is a ceramic film with a 50nm film core.
Preferably, the microwave treatment in step S12 is performed at a microwave power of 250-400w for a treatment time of 10-14 mi. More preferably, the microwave treatment in step S12 is performed at a microwave power of 300w for a treatment time of 12 mi.
Preferably, the ultrasonic treatment in step S12 is performed at an ultrasonic power of 150-250w, an ultrasonic frequency of 25Hz, and a treatment time of 11-15 mi. More preferably, the ultrasonic treatment is carried out at an ultrasonic power of 200w for a treatment time of 14 mi.
Preferably, the ceramic film described in step S13 is a 50nm film core ceramic film.
Preferably, the ultrafiltration membrane described in step S13 is an ultrafiltration membrane having a molecular weight cut-off of 1000 to 10000 daltons (Da). More preferably, the ultrafiltration membrane is an ultrafiltration membrane having a molecular weight cut-off of 5000 daltons.
Preferably, in the step S22, the freezing temperature is-10 ℃, the reaction time in the step S23 is 4 hours, and the dialysis time is 24 hours.
Preferably, in the step S44, the stirring time is 3 hours, and the stirring speed is 500 revolutions per minute.
The invention also provides application of the matrimony vine polysaccharide and matrimony vine polysaccharide-matrimony vine seed oil soft capsule obtained by the method in preparation of drugs for improving antioxidant activity, improving immunity and reducing blood sugar.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of lycium barbarum polysaccharide, which utilizes the combination of a microwave-assisted ultrasonic water-soluble extraction method and a ceramic membrane-ultrafiltration membrane separation technology to extract the lycium barbarum polysaccharide. The wolfberry polysaccharide prepared by the method has high extraction rate up to more than 70%, high biological activity and good quality; the ceramic membrane-ultrafiltration membrane separation effect is good in the extraction process, the membrane core is stable in operation, the filtration yield is high, the anti-fouling performance is strong, the cleaning and recovery are easy, and the method is suitable for industrial mass production.
In addition, the wolfberry polysaccharide obtained by the preparation method provided by the invention has remarkable in-vitro antioxidant activity, improves immunity and restores physiological effects of cells, and can be used for reducing blood sugar and preventing and treating diabetes.
As the wolfberry polysaccharide molecules have hydrophilicity and are oleophobic molecules, the wolfberry polysaccharide molecules cannot be well combined with the wolfberry seed oil, a large number of hydroxyl groups are contained in the wolfberry polysaccharide molecular chain, after acetic anhydride is added, the hydroxyl groups in the wolfberry polysaccharide react with the acetic anhydride, acetyl groups are obtained on the wolfberry polysaccharide, so that the surface activity of the wolfberry polysaccharide is enhanced, the wolfberry polysaccharide has lipophilic groups, the emulsifying performance of the wolfberry polysaccharide is enhanced, and the wolfberry polysaccharide can be well combined with the wolfberry seed oil in an emulsifying way.
In the invention, in order to not influence the oxidation activity of the oxidation group of the medlar, the added acetyl group enables the quantity of the hydroxyl groups replaced by the acetyl groups in the medlar polysaccharide to be about 8-10%, and proper acetyl groups are added into the medlar polysaccharide to improve the emulsifying property of the medlar polysaccharide. Meanwhile, in order to improve the activity of the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule, under the condition that the combining capability of the lycium barbarum polysaccharide-lycium barbarum seed oil is not affected, a certain amount of carboxymethyl is added to the lycium barbarum polysaccharide, so that the hydroxyl is replaced by carboxymethyl, the substitution degree is about 5-10%, and the capability of the lycium barbarum polysaccharide-lycium barbarum seed oil in the characteristics of immunoregulation, antioxidation and the like is improved.
Although a small amount of acetyl groups are added into the polysaccharide, the emulsifying performance is improved, but the activity of the wolfberry polysaccharide is reduced to a certain extent, so that a certain amount of carboxymethyl is added onto the wolfberry polysaccharide on the basis of adding the acetyl groups, and the activity of the wolfberry polysaccharide is improved, but because the carboxymethyl is a hydrophilic group, the emulsifying performance is reduced compared with that of the wolfberry polysaccharide with the single acetyl group, while the activity of the wolfberry polysaccharide is improved, and therefore, a certain amount of sorbitan monooleate is added in the mixing process of the wolfberry polysaccharide and the wolfberry seed oil.
According to the invention, sorbitan monooleate is added when the wolfberry polysaccharide and the wolfberry seed oil are mixed, so that the wolfberry polysaccharide and the wolfberry seed oil are completely fused, the wolfberry polysaccharide-wolfberry seed oil mixture can be prevented from settling, layering and flocculation of the wolfberry polysaccharide-wolfberry seed oil are prevented, and the wolfberry polysaccharide-wolfberry seed oil capsule prepared by the method has high rationality and lower production cost.
As the invention reasonably prepares the acetyl substitution amount, the carboxymethyl substitution amount and the addition amount of the sorbitan monooleate of the lycium barbarum polysaccharide, the proportion of the lycium barbarum polysaccharide to the lycium barbarum seed oil can reach 1:1, and the proportion of the lycium barbarum polysaccharide to the lycium barbarum seed oil soft capsule prepared by the conventional method is generally less than 35 percent.
Drawings
FIG. 1 is a flow chart of a preparation method of a Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule;
FIG. 2 is a flowchart of the extraction process of the Lycium barbarum polysaccharide in step S1;
FIG. 3 is a flow chart of the molecular modification of the Lycium barbarum polysaccharide in step S2;
FIG. 4 is a flow chart of the preparation of the wolfberry polysaccharide-wolfberry seed oil soft capsule in step S4;
FIG. 5 shows a gel permeation chromatography of an ultrafiltration membrane with a molecular weight cutoff of 1000Da for extracting Lycium barbarum polysaccharide;
FIG. 6 is a gel permeation chromatogram of Lycium barbarum polysaccharide passing through ultrafiltration membrane with molecular weight cutoff of 3000 Da;
FIG. 7 is a gel permeation chromatography of Lycium barbarum polysaccharide through an ultrafiltration membrane with a molecular weight cutoff of 5000 Da;
FIG. 8 is a gel permeation chromatography of Lycium barbarum polysaccharide through an ultrafiltration membrane with a molecular weight cutoff of 10000 Da.
Detailed Description
Next, embodiments of the present invention will be described.
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
The preparation method of the wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4, preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule.
S1, extracting wolfberry polysaccharide, which comprises the following steps:
s11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing, sieving, and sieving with a 40-mesh sieve to obtain Chinese wolfberry powder;
s12, 10000g of medlar powder obtained in the step S11 is taken, purified water is added according to the ratio of 1:6, microwave treatment is carried out at normal temperature, the microwave power is 250w, and the treatment time is 10min; then carrying out ultrasonic treatment, wherein the ultrasonic power is 150w, the ultrasonic frequency is 25Hz, the treatment time is 11min, filtering is carried out, and the filtrate is collected;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane with a 50nm membrane core for 100min, wherein the inlet and outlet pressure is 2.8/1.9Bar, the treatment temperature is 38 ℃, filtering and concentrating, then passing through an ultrafiltration membrane with a molecular weight cut-off of 5000 daltons, filtering and concentrating again, the treatment time is 25min, the inlet and outlet pressure is 2/2Bar, the treatment temperature is 15 ℃, and collecting concentrated solution;
s14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide;
s2, modifying wolfberry polysaccharide molecules, which comprises the following steps:
s21, adding 316g of medlar polysaccharide into 3160g of formamide organic solvent according to mass fraction, adding 632g of pyridine, stirring and mixing thoroughly, and adding 316g of acetic anhydride;
S22, stirring the materials obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying at the temperature of minus 10 ℃ to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 316g of the wolfberry polysaccharide obtained in the step S1, adding 4740g of formamide solvent, stirring for 1.5 hours, adding 1580g of 20% sodium hydroxide aqueous solution, simultaneously adding 948g of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 24 hours by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the wolfberry polysaccharide containing acetyl and carboxymethyl;
s3, extracting medlar seed oil, which comprises the following steps:
s31, rinsing and sun-drying the wolfberry residues after the wolfberry polysaccharide is extracted, controlling the water content to be less than or equal to 5%, crushing the wolfberry residues by a ten-thousand-level crusher, and crushing the wolfberry seeds to 30 meshes.
S32, supercritical extraction: liquid CO with flow rate of 550L/min is pumped by a high-pressure pump at 28MPa 2 Pumping into extraction kettle, mixing with fructus Lycii seed, and extracting under supercritical state at 33deg.C.
S33, separation: the temperature of the separation kettle is raised to 40-45 ℃ and the pressure is controlled to 10-12MPa, so that the carbon dioxide is changed from a liquid state to a gaseous state, and is separated from the medlar seed oil and recycled.
S34, filtering: the separated medlar seed oil is filtered by a rectifying kettle, and impurities in the medlar seed oil are filtered out by adopting 300-mesh filter cloth and stored in a storage tank temporarily.
S4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, which comprises the following steps:
s41, preparing the wolfberry polysaccharide obtained in the step S2 into 50% wolfberry polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: weighing the wolfberry polysaccharide obtained in the step S2 and the wolfberry seed oil obtained in the step S3 according to the proportion of 1:1, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device;
s43, adding sorbitan monooleate accounting for 3% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
s45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Example 2
The preparation method of the wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4 preparation of Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule
S1, extracting wolfberry polysaccharide, which comprises the following steps:
s11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing, sieving, and sieving with a 40-mesh sieve to obtain Chinese wolfberry powder;
s12, 10000g of medlar powder obtained in the step S11 is taken, purified water is added according to the ratio of 1:5, microwave treatment is carried out at normal temperature, the microwave power is 400w, and the treatment time is 14min; then carrying out ultrasonic treatment, wherein the ultrasonic power is 250w, the ultrasonic frequency is 25Hz, the treatment time is 15min, filtering is carried out, and the filtrate is collected;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane with a 50nm membrane core for 500min, wherein the inlet and outlet pressure is 2.8/1.9Bar, the treatment temperature is 45 ℃, filtering and concentrating, then passing through an ultrafiltration membrane with a molecular weight cut-off of 1000 daltons, filtering and concentrating again, the treatment time is 225min, the inlet and outlet pressure is 35/34.5Bar, the treatment temperature is 39 ℃, and collecting concentrated solution;
s14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide;
S2, modifying wolfberry polysaccharide molecules, which comprises the following steps:
s21, adding 294g of medlar polysaccharide into 3230g of formamide organic solvent according to mass fraction, adding 73g of pyridine, stirring and mixing thoroughly, and adding 310g of acetic anhydride;
s22, stirring the material obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 294g of the wolfberry polysaccharide obtained in the step S1, adding 470g of formamide solvent, stirring for 2 hours, adding 1760g of 20% sodium hydroxide aqueous solution, simultaneously adding 1000g of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 20 hours by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the wolfberry polysaccharide containing acetyl and carboxymethyl;
s3, extracting medlar seed oil, which comprises the following steps:
s31, rinsing and sun-drying the wolfberry residues after the wolfberry polysaccharide is extracted, controlling the water content to be less than or equal to 5%, crushing the wolfberry residues by a ten-thousand-level crusher, and crushing the wolfberry seeds to 30 meshes.
S32, supercritical extraction: liquid CO with flow rate of 550L/min is pumped by a high-pressure pump at 28MPa 2 Pumping into extraction kettle, mixing with fructus Lycii seed, and extracting under supercritical state at 33deg.C.
S33, separation: the temperature of the separation kettle is raised to 40-45 ℃ and the pressure is controlled to 10-12MPa, so that the carbon dioxide is changed from a liquid state to a gaseous state, and is separated from the medlar seed oil and recycled.
S34, filtering: the separated medlar seed oil is filtered by a rectifying kettle, and impurities in the medlar seed oil are filtered out by adopting 300-mesh filter cloth and stored in a storage tank temporarily.
S4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, which comprises the following steps:
s41, preparing the wolfberry polysaccharide obtained in the step S2 into 65% wolfberry polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: the medlar seed oil is 1:1.2, medlar polysaccharide obtained in the step S2 and medlar seed oil obtained in the step S3 are weighed, and the weighed medlar polysaccharide and medlar seed oil are added into a mixing and stirring device;
s43, adding sorbitan monooleate accounting for 4% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
S45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Example 3
The preparation method of the wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4 preparation of Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule
S1, extracting wolfberry polysaccharide, which comprises the following steps:
s11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing, sieving, and sieving with a 40-mesh sieve to obtain Chinese wolfberry powder;
s12, 10000g of medlar powder obtained in the step S11 is taken, purified water is added according to the ratio of 1:7, and microwave treatment is carried out at normal temperature, wherein the microwave power is 300w, and the treatment time is 12min; then carrying out ultrasonic treatment, wherein the ultrasonic power is 200w, the ultrasonic frequency is 25Hz, the treatment time is 14min, filtering is carried out, and the filtrate is collected;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane with a 50nm membrane core for 350min, wherein the inlet and outlet pressure is 2.8/1.9Bar, the treatment temperature is 46 ℃, filtering and concentrating, then passing through an ultrafiltration membrane with a molecular weight cutoff of 3000 daltons, filtering and concentrating again, the treatment time is 80min, the inlet and outlet pressure is 6/5.5Bar, the treatment temperature is 28 ℃, and collecting concentrated solution;
S14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide;
s2, modifying wolfberry polysaccharide molecules, which comprises the following steps:
s21, adding 258g of extracted wolfberry polysaccharide into 3010g of formamide organic solvent according to mass fraction, adding 594g of pyridine, stirring and mixing thoroughly, and adding 260g of acetic anhydride;
s22, stirring the material obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 31.6g of the lycium barbarum polysaccharide obtained in the step S1, adding 3870g of formamide solvent, stirring for 1.5h, adding 1420g of 20% sodium hydroxide aqueous solution, simultaneously adding 9480g of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 10 h by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the lycium barbarum polysaccharide containing acetyl and carboxymethyl;
s3, extracting medlar seed oil, which comprises the following steps:
s31, rinsing and sun-drying the wolfberry residues after the wolfberry polysaccharide is extracted, controlling the water content to be less than or equal to 5%, crushing the wolfberry residues by a ten-thousand-level crusher, and crushing the wolfberry seeds to 30 meshes.
S32, supercritical extraction: liquid CO with flow rate of 550L/min is pumped by a high-pressure pump at 28MPa 2 Pumping into extraction kettle, mixing with fructus Lycii seed, and extracting under supercritical state at 33deg.C.
S33, separation: the temperature of the separation kettle is raised to 40-45 ℃ and the pressure is controlled to 10-12MPa, so that the carbon dioxide is changed from a liquid state to a gaseous state, and is separated from the medlar seed oil and recycled.
S34, filtering: the separated medlar seed oil is filtered by a rectifying kettle, and impurities in the medlar seed oil are filtered out by adopting 300-mesh filter cloth and stored in a storage tank temporarily.
S4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, which comprises the following steps:
s41, preparing the medlar polysaccharide obtained in the step S2 into 45% medlar polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: the medlar seed oil is 1:1.1, medlar polysaccharide obtained in the step S2 and medlar seed oil obtained in the step S3 are weighed, and the weighed medlar polysaccharide and medlar seed oil are added into a mixing and stirring device;
s43, adding sorbitan monooleate accounting for 5% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
S45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Example 4
The preparation method of the wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4 preparation of Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule
S1, extracting wolfberry polysaccharide, which comprises the following steps:
s11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing, sieving, and sieving with a 40-mesh sieve to obtain Chinese wolfberry powder;
s12, 10000g of medlar powder obtained in the step S11 is taken, purified water is added according to the ratio of 1:5, microwave treatment is carried out at normal temperature, the microwave power is 400w, and the treatment time is 14min; then carrying out ultrasonic treatment, wherein the ultrasonic power is 250w, the ultrasonic frequency is 25Hz, the treatment time is 15min, filtering is carried out, and the filtrate is collected;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane with a 50nm membrane core for 500min, wherein the inlet and outlet pressure is 2.8/1.9Bar, the treatment temperature is 45 ℃, filtering and concentrating, then passing through an ultrafiltration membrane with a molecular weight cutoff of 10000 daltons, filtering and concentrating again, the treatment time is 225min, the inlet and outlet pressure is 35/34.5Bar, the treatment temperature is 39 ℃, and collecting concentrated solution;
S14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide;
s2, modifying wolfberry polysaccharide molecules, which comprises the following steps:
s21, adding 227g of medlar polysaccharide into 2270g of formamide organic solvent according to mass fraction, adding 45.4 pyridine, stirring and mixing thoroughly, and adding 227g of acetic anhydride;
s22, stirring the material obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 31.6g of the lycium barbarum polysaccharide obtained in the step S1, adding 3410g of formamide solvent, stirring for 1.5h, adding 1200g of 20% sodium hydroxide aqueous solution, simultaneously adding 682g of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 20 h by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the lycium barbarum polysaccharide containing acetyl and carboxymethyl;
s3, extracting medlar seed oil, which comprises the following steps:
s31, rinsing and sun-drying the wolfberry residues after the wolfberry polysaccharide is extracted, controlling the water content to be less than or equal to 5%, crushing the wolfberry residues by a ten-thousand-level crusher, and crushing the wolfberry seeds to 30 meshes.
S32, supercritical extraction: liquid CO with flow rate of 550L/min is pumped by a high-pressure pump at 28MPa 2 Pumping into extraction kettle, mixing with fructus Lycii seed, and extracting under supercritical state at 33deg.C.
S33, separation: the temperature of the separation kettle is raised to 40-45 ℃ and the pressure is controlled to 10-12MPa, so that the carbon dioxide is changed from a liquid state to a gaseous state, and is separated from the medlar seed oil and recycled.
S34, filtering: the separated medlar seed oil is filtered by a rectifying kettle, and impurities in the medlar seed oil are filtered out by adopting 300-mesh filter cloth and stored in a storage tank temporarily.
S4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, which comprises the following steps:
s41, preparing the wolfberry polysaccharide obtained in the step S2 into 40% wolfberry polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: weighing the wolfberry polysaccharide obtained in the step S2 and the wolfberry seed oil obtained in the step S3 according to the proportion of 1:0.8, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device;
s43, adding sorbitan monooleate accounting for 3% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
S45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Comparative example
Comparative experiments were carried out on the basis of example 1, and the prepared Lycium barbarum polysaccharide-Lycium barbarum seed oil capsules have certain differences in the absence of certain additives, and part of the comparative examples are listed below.
Comparative example 1
The present comparative example differs from example 1 in step S2, in that the present comparative example step S2 does not have steps S21 and S22 in example one, but only step S23 in example 1, and other steps are the same as example 1, and the present comparative example step S2 is specifically:
s23, taking 316g of the wolfberry polysaccharide obtained in the step S1, adding 4740g of formamide solvent, stirring for 1.5h, adding 1580g of 20% sodium hydroxide aqueous solution, simultaneously adding 948g of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 24 h by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain the wolfberry polysaccharide containing acetyl and carboxymethyl;
4. the substitution degree distribution of carboxymethyl in the polysaccharide is 0.094 measured by an infrared spectrum analysis method;
comparative example 2
The present comparative example differs from example 1 in step S2, the present comparative example does not have step S23 in example 1, only steps S21, S22 in example 1, and other steps are the same as example 1, and the present comparative example step S2 is specifically:
s21, adding 316g of medlar polysaccharide into 3160g of formamide organic solvent according to mass fraction, adding 632 pyridine, stirring and mixing thoroughly, and adding 316g of acetic anhydride;
s22, stirring the materials obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying at the temperature of minus 10 ℃ to obtain the lycium barbarum polysaccharide with acetyl groups;
comparative example 3
The present comparative example differs from example 1 in step S4, and the present comparative example does not have step c of step S4 in example 1, and other steps are the same as example 1, and the present comparative example step S4 is specifically:
s41, preparing the wolfberry polysaccharide obtained in the step S2 into 50% wolfberry polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: weighing the wolfberry polysaccharide obtained in the step S2 and the wolfberry seed oil obtained in the step S3 according to the proportion of 15:100, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
S44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
s45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Comparative example 4
This comparative example differs from example 1 in that there is no polysaccharide molecule modification step S2, and the other steps are the same as example 1, specifically:
extracting Lycium barbarum polysaccharide;
s3, extracting medlar seed oil;
s4, preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule.
Comparative example 5
This comparative example differs from example 1 in that there is no modification of the lycium barbarum polysaccharide molecule at step S2 of example 1, and in that there is no step S43 of example 1 at step S4, otherwise the same as example 1, specifically:
s1, extracting wolfberry polysaccharide;
s2, extracting medlar seed oil;
s4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule:
s41, preparing the wolfberry polysaccharide obtained in the step S2 into 50% wolfberry polysaccharide water solution
S42, preparing a medlar polysaccharide water solution according to the mass ratio: weighing the wolfberry polysaccharide obtained in the step S2 and the wolfberry seed oil obtained in the step S3 according to the proportion of 1:1, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
S44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
s45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
Examples and comparative examples results testing and analysis:
the Lycium barbarum polysaccharide extracts and the Lycium barbarum polysaccharide-Lycium barbarum seed oil mixture samples obtained in the above examples and comparative examples were analyzed.
1. Sensory index evaluation
Sensory index evaluation was performed on the wolfberry polysaccharide obtained in examples 1-4, and the wolfberry polysaccharide obtained in examples 1-4 meets the requirements of Table 1.
Table 1: sensory average requirement of Lycium barbarum polysaccharide
2. Molecular weight analysis of Lycium barbarum polysaccharide sample
The detection method comprises the following steps: gel Permeation Chromatography (GPC);
chromatographic conditions: three columns of UltraHydromdl, guard column and Ultrahydrogdl lindr are connected in series; mobile phase 100mM NaNO 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate is 0.6mL/min; the temperature is 35 ℃;
standard substance: ddxtran (dextran), molecular weight: 11.6-668kDa.
The gel permeation chromatography of examples 1-4 is obtained, and figures 5-8 are gel permeation chromatography of ultrafiltration membranes with standard substance passing through molecular weight cut-off of 1000Da, 3000Da, 5000Da and 10000Da respectively, and can be used as internal control standard to verify process stability and molecular weight distribution of target product.
The wolfberry polysaccharide obtained in examples 1-4 was tested, and the results showed that: the peaks of the four samples with different molecular weights at different positions are basically similar, and the molecular weight distribution condition of the internal control standard map is met, which shows that the ceramic membrane-ultrafiltration membrane separation effect is good in the extraction process.
3. Lycium barbarum polysaccharide yield and weight scale of Lycium barbarum polysaccharide powder
Detecting the content of the Lycium barbarum polysaccharide after ultrafiltration in examples 1-4, and calculating the yield; the resulting wolfberry polysaccharide powder was weighed and the results are shown in Table 2.
Table 2: lycium barbarum polysaccharide yield and weight scale of Lycium barbarum polysaccharide powder
| Experimental sample | Ultrafiltration of Lycium barbarum polysaccharide yield | Matrimony vine polysaccharide powder weight (g) |
| Example 1 | 85.7％ | 316 |
| Example 2 | 82.4％ | 294 |
| Example 3 | 79.8％ | 258 |
| Example 4 | 77.6％ | 227 |
As can be seen from the results in Table 2, the wolfberry polysaccharide prepared by the preparation method provided by the invention has high content, and the filtration yield of the ceramic membrane-ultrafiltration membrane system used is high.
4. Analysis of substitution degree of Lycium barbarum polysaccharide group
The substitution degree of acetyl and carboxymethyl in the wolfberry polysaccharide is measured by utilizing an infrared spectrum analysis method, the substitution amount of hydroxyl groups to acetyl and carboxymethyl is measured by utilizing the infrared spectrum absorption peak height, the substitution degree of acetyl is calculated by utilizing a formula DS=162A/4300-42A, and the substitution degree of carboxymethyl is calculated by utilizing a formula DS=0.162A/1-0.058A. In examples and comparative examples, the degrees of substitution of acetyl groups and carboxymethyl groups in the Lycium barbarum polysaccharide are shown in Table 3.
Table 3: degree of substitution of acetyl and carboxymethyl groups in Lycium barbarum polysaccharide
| Experimental sample | Degree of substitution of acetyl group in Lycium barbarum polysaccharide | Degree of substitution of carboxymethyl group in Lycium barbarum polysaccharide |
| Example 1 | 0.093 | 0.073 |
| Examples2 | 0.079 | 0.103 |
| Example 3 | 0.085 | 0.086 |
| Example 4 | 0.101 | 0.052 |
| Comparative example 1 | / | 0.094 |
| Comparative example 2 | 0.132 | / |
As is clear from Table 3, examples 1, comparative example 1 and comparative example 2, the acetyl groups and carboxymethyl groups in the Lycium barbarum polysaccharide affect the degree of substitution of the different groups in the Lycium barbarum polysaccharide.
5. Evaluation of viscosity and emulsion stability of Lycium Barbarum polysaccharide, lycium Barbarum polysaccharide-Lycium Barbarum seed oil mixture
In order to average the emulsifying property of the lycium barbarum polysaccharide-lycium barbarum seed oil mixture and the emulsifying property of the modified group on the lycium barbarum polysaccharide, the emulsifying property of the lycium barbarum polysaccharide obtained in different steps and the lycium barbarum polysaccharide-lycium barbarum seed oil mixture in example 1 and comparative example was evaluated. The emulsion performance of the lycium barbarum polysaccharide was evaluated by liquid interfacial tension measurement, and in the test, the lycium barbarum polysaccharide was formulated as a 50% aqueous solution of lycium barbarum polysaccharide. The stability of the content of Lycium barbarum polysaccharide-Lycium barbarum seed oil is evaluated by maintaining at 25deg.C for 7 days, and testing the surface tension of the solution, as shown in Table 4.
Table 4 surface tension of Lycium barbarum polysaccharide obtained by different steps and surface Zhang Libiao of Lycium barbarum polysaccharide-Lycium barbarum seed oil Soft Capsule content
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As can be seen from Table 4, after the acetyl modification of the Lycium barbarum polysaccharide molecule, the surface tension is reduced, and the addition of the acetyl group improves the emulsifying property of the Lycium barbarum polysaccharide molecule, but after the addition of the carboxymethyl, the surface tension of the Lycium barbarum polysaccharide is increased, which indicates that after the carboxymethyl is added to the Lycium barbarum polysaccharide molecule, the emulsifying property of the Lycium barbarum is reduced, and in the step S4, the surface tension of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule content is very small after the sorbitan monooleate is added, the surface Lycium barbarum polysaccharide and the Lycium barbarum seed oil are fully fused, and after the sorbitan monooleate is added, the stability of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule content is better, and after the carboxymethyl is added, the observed Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule content is uniformly mixed, and no flocculation or layering substances appear after the mixture is left for 7 days.
In comparative example 1, no acetyl group was added, but sorbitan monooleate was added, but the mixture of lycium barbarum polysaccharide and lycium barbarum seed oil was not fused well, and after the mixture was completed, a bubble phenomenon was observed, and after 7 days, a layered flocculation phenomenon occurred.
Comparative example 2, in which no carboxymethyl group was added, but acetyl group and sorbitan monooleate were added, the Lycium barbarum polysaccharide-Lycium barbarum seed oil fusion degree was good.
In comparative example 3, sorbitan monooleate was not added, but acetyl and carboxymethyl were added, and the initial fusion degree of Lycium barbarum polysaccharide-Lycium barbarum seed oil was good, but the stability was poor, and a layering flocculation phenomenon occurred after 7 days.
In comparative example 4, acetyl and carboxymethyl are not added, but sorbitan monooleate is added, and the initial fusion degree of the lycium barbarum polysaccharide-lycium barbarum seed oil is good, but the stability is poor, and the layering flocculation phenomenon occurs after 7 days.
In comparative example 5, without addition of acetyl, carboxymethyl and sorbitan monooleate, the polysaccharide-seed oil could not be mixed and after stopping stirring, the tendency to delaminate began to appear.
6. Lycium barbarum polysaccharide, lycium barbarum polysaccharide-Lycium barbarum seed oil content viscosity test
In the viscosity test, the viscosity of the wolfberry polysaccharide obtained by different steps after the wolfberry polysaccharide and the wolfberry polysaccharide are modified and the viscosity of the content of the wolfberry polysaccharide-wolfberry seed oil soft capsule is tested by preparing the wolfberry polysaccharide into 50 mass percent of wolfberry polysaccharide aqueous solution, and the viscosity of the content of the wolfberry polysaccharide-wolfberry seed oil soft capsule is shown in Table 5 in detail.
TABLE 5 viscosity of aqueous solution of Lycium barbarum polysaccharide obtained by various steps and viscosity of Lycium barbarum polysaccharide-Lycium barbarum seed oil
As can be seen from Table 5, the viscosity of the Lycium barbarum polysaccharide increases after the addition of the acetyl group, and the viscosity of the Lycium barbarum polysaccharide decreases after the addition of the carboxymethyl group to the Lycium barbarum polysaccharide, and the viscosity of the Lycium barbarum polysaccharide-Lycium barbarum seed oil mixture after the addition of the sorbitan monooleate is significantly greater than that of the Lycium barbarum polysaccharide-Lycium barbarum seed oil mixture without the addition of the sorbitan monooleate.
7. Lycium barbarum polysaccharide and Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule antioxidant activity detection method
The biological activity of Lycium barbarum polysaccharides is mainly antioxidant activity, and oxidation free radical absorption capacity (ORAC) is also called antioxidant capacity. The ORAC analysis method is based on the principle that the free radical breaks down the fluorescent probe to change the fluorescence intensity, and uses the vitamin d water-soluble analogue Trolox as a quantitative standard to analyze by using a fluorescent microplate analyzer. The magnitude of the change in fluorescence intensity reflects the degree of free radical destruction. In the presence of an antioxidant, it can inhibit the change in fluorescence caused by free radicals to the extent that reflects its antioxidant capacity towards free radicals.
ORAC detection was performed on the Lycium barbarum polysaccharides obtained in examples 1-4, and the results are shown in Table 6.
Table 6: detection of Lycium barbarum polysaccharide and Lycium barbarum polysaccharide-Lycium barbarum seed oil Soft Capsule ORAC
The ORAC method measurement results show that: the wolfberry polysaccharide product obtained by the invention has strong oxidation resistance and high biological activity. After acetyl is added into the wolfberry polysaccharide molecules, the oxidation resistance of the wolfberry polysaccharide is weakened to a certain extent, after carboxymethyl is added into the wolfberry polysaccharide molecules on the basis of adding acetyl, the oxidation resistance of the wolfberry polysaccharide is improved, after sorbitan monooleate is added, the oxidation resistance structure of the wolfberry polysaccharide-wolfberry seed oil soft capsule content is more stable, and presumably, the result that the wolfberry polysaccharide and the wolfberry seed oil can be fully mixed after the sorbitan monooleate is added is obtained.
8. Detection of influence of matrimony vine polysaccharide-matrimony vine seed oil soft capsule resistance on immunosuppressed mouse spleen lymphocyte proliferation
Male adult ICR mice weighing 18-22g were selected for clean-grade rearing for one week to adapt to the environment and eliminate stress response. The food is fasted for 12 hours in the night before molding, and water is not forbidden. Daily morning, fasted mice were weighed and fed continuously for 21 days with Lycium barbarum polysaccharide obtained in different steps. After 24h of last dose, 5 mice per group were sacrificed at random, the orbit was bled, whole blood and serum was collected and stored at-20 ℃. The peritoneal macrophages and spleen lymphocytes are taken aseptically for later use, and the remaining 5 cells are continuously administered for 7 days, and the sample is collected according to the same method. Mice were sacrificed by eye drop exsanguination, spleens were removed, and surrounding tissues were peeled clean and weighed.
After the administration period is finished, the cervical vertebra dislocation of all experimental mice is killed, the mice are soaked in 75% alcohol for 5min, the spleens are removed aseptically, the mice are immediately placed in a culture dish containing a proper amount of RPMI-1640 basic culture medium without serum, and the mice are washed for 2-3 times by the culture medium, so that blood stains are washed. Cutting the washed spleen into small pieces by scissors, lightly transferring the small pieces into a 200-mesh stainless steel filter screen, lightly grinding the small pieces, flushing the filter screen with RPMI-1640 culture medium without serum for 1-2 times, collecting cell suspension, centrifuging for 10min at 1000g, discarding supernatant, adding 5mL of Tris-NH4Cl (pH 7.4) solution for lysing red blood cells for reacting for 5min, centrifuging for 10min at 200g, and discarding supernatant. After washing three times with PBS buffer solution, adding RPMI-1640 complete culture medium (containing 10% eBS and 1% double antibody) to resuspend cells, lightly blowing the cells with a pipette gun, counting with 0.4% trypan blue solution, and adjusting the cell concentration to 5X 106 cells/mL to obtain spleen lymphocyte suspension.
The prepared spleen lymphocyte suspension is fully and uniformly mixed and then added into a 96-well cell plate (100 mu L/well), the 96-well cell plate is gently shaken for 3min to uniformly mix cells, and the spleen lymphocyte suspension is divided into a test group and a control group, wherein each group is provided with three compound wells. Concanavalin A (ConA) and Lipopolysaccharide (LPS) were added to the test groups at a final concentration of 5. Mu.g/mL and at a final concentration of 10. Mu.g/mL, respectively, in a total volume of 200. Mu.L per well, with RPMI 1640 basal medium without serum as a blank. The plates were placed in a 37℃5% CO2 incubator for 66h incubation, the incubation was terminated, 20. Mu.L of MTT (1 mg/L) was added to each well, incubation was continued for 4h, the reaction was terminated, the medium was pipetted off, 100. Mu.L of dimethyl sulfoxide (DMSO) was added, and the shaker was oscillated for 5min, and the OD of each well was measured at λ=570 nm using an automatic microplate reader.
The proliferation rate of splenic lymphocytes was calculated according to the following formula:
the obtained data of the influence of the content of Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule on immunosuppression of mouse spleen lymphocyte proliferation are shown in Table 7
TABLE 7 immune suppression of spleen lymphocyte proliferation rate in mice by Lycium barbarum polysaccharide obtained by various steps
The proliferation rate of T lymphocyte proliferation and B lymphocyte proliferation induced by acetyl-treated Lycium barbarum polysaccharide of comparative example 2 is significantly reduced compared with example 1, which indicates that comparative example 2 can cause obvious damage to the proliferation capacity of spleen lymphocytes of mice. Comparative example 1, without acetyl treatment, was directly subjected to carboxymethyl treatment of lycium barbarum polysaccharide, and proliferation rates of T lymphocyte proliferation and B lymphocyte proliferation induced by lycium barbarum polysaccharide were both significantly increased, indicating that lycium barbarum polysaccharide and carboxymethyl lycium barbarum polysaccharide can enhance body immune function by promoting immunosuppression of mouse spleen lymphocyte proliferation.
In addition, in the invention, some comparative experiments are carried out, for example, in order to achieve the emulsification effect and the emulsification stability of the content of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule of the embodiment 1 on the basis of the comparative example 1, sorbitan monooleate which is about 10% of the total mass of the content of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule is also required to be added on the basis of the comparative example 1, but the ORAC value of the obtained product is 457+/-2 mu molds Td/g when the oxidation resistance is detected, and is obviously lower than the ORAC value of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule obtained in the embodiment 1.
In order to achieve the emulsifying effect and the emulsifying stability of the content of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule of the embodiment 1, the acetyl substitution degree of the Lycium barbarum polysaccharide is 0.34 on the basis of the comparative example 3, but the ORAC value of the obtained product is 476+/-2 mu molds Td/g when the oxidation resistance is detected, which is obviously lower than that of the Lycium barbarum polysaccharide-Lycium barbarum seed oil soft capsule of the embodiment 1.
In addition, in some embodiments of the present invention, in order to achieve the specific technical effect of the experimental apparatus, a person skilled in the art may perform specific parameter setting through common general knowledge, and in embodiments, details such as drying process temperature and time, water extraction temperature and time, stirring speed and stirring time are not required.
As can be seen from the above examples and comparative analyses,
the wolfberry polysaccharide prepared by the preparation method provided by the invention has high extraction rate which can reach more than 70%, strong oxidation resistance, high biological activity and good quality; the ceramic membrane-ultrafiltration membrane separation effect is good in the extraction process, the membrane core is stable in operation, the filtration yield is high, the anti-fouling performance is strong, the cleaning and recovery are easy, and the method is suitable for industrial mass production.
Under the premise of not affecting the emulsion stability and the antioxidation capability of the content of the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule, the acetyl substitution degree and the carboxymethyl substitution degree of the lycium barbarum polysaccharide cannot be too high, and the addition amount of the sorbitan monooleate cannot be too low, otherwise, the dispersion and fusion capability and the bioactivity of the lycium barbarum polysaccharide-lycium barbarum seed oil are affected.
The optimal acetyl substitution degree of the matrimony vine polysaccharide is 8-10%, the optimal carboxymethyl substitution degree of the matrimony vine polysaccharide is 5-10%, and the optimal amount of the sorbitan monooleate added is 3-5% of the total mass of the matrimony vine polysaccharide-matrimony vine seed oil soft capsule content.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced with equivalents; such modifications and substitutions do not depart from the spirit of the technical solutions according to the embodiments of the present invention.
Claims (5)
1. A preparation method of a wolfberry polysaccharide-wolfberry seed oil soft capsule comprises the following steps: s1, extracting wolfberry polysaccharide; s2, modifying wolfberry polysaccharide molecules; s3, extracting medlar seed oil; s4, preparing a wolfberry polysaccharide-wolfberry seed oil soft capsule, wherein the step S1 of extracting wolfberry polysaccharide comprises the following steps:
S11, screening dried fruits or fresh fruits of the Chinese wolfberry, removing impurities and diseased fruits, cleaning, drying, crushing and sieving to obtain Chinese wolfberry powder;
s12, mixing the medlar powder obtained in the step S11 according to a feed liquid ratio of 1: purified water is added in a ratio of 5 to 1:7, microwave treatment is carried out at normal temperature, then ultrasonic treatment is carried out, filtration is carried out, and filtrate is collected;
s13, passing the filtrate obtained in the step S12 through a ceramic membrane for 100min at a pressure of 2.8/1.9Bar, filtering and concentrating at 38 ℃, passing through an ultrafiltration membrane for further filtering and concentrating for 25min at a pressure of 2/2Bar, and collecting the concentrated solution at a temperature of 15 ℃;
s14, freeze-drying the concentrated solution obtained in the step S13, and crushing at a low temperature to obtain the lycium barbarum polysaccharide;
the S2 wolfberry polysaccharide molecule modification comprises the following steps:
s21, adding 10 parts of medlar polysaccharide extracted in the step S1 into 100 parts of formamide organic solvent according to mass fraction, adding 2 parts of pyridine, stirring and mixing thoroughly, and adding 10 parts of acetic anhydride;
s22, stirring the material obtained in the step S21 for 12 hours at normal temperature, dialyzing and concentrating, and freeze-drying to obtain the lycium barbarum polysaccharide with acetyl groups;
s23, taking 10 parts of the medlar polysaccharide with acetyl groups obtained in the step S22, adding 150 parts of formamide solvent, stirring for 1.5 hours, adding 5 parts of 20% sodium hydroxide aqueous solution, simultaneously adding 3 parts of chloroacetic acid, stirring, reacting at 70 ℃, dialyzing for 24 hours by using a distilled water dialysis bag after the reaction is finished, and freeze-drying after the dialysis is finished to obtain medlar polysaccharide containing acetyl groups and carboxymethyl groups;
The substitution degree of acetyl in the wolfberry polysaccharide is 8-10%, and the substitution degree of carboxymethyl is 5-10%;
the S4 lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule is prepared by the following steps:
s41, preparing the lycium barbarum polysaccharide obtained in the step S2 into a lycium barbarum polysaccharide aqueous solution with the concentration of 40% -65%;
s42, according to the mass fraction ratio of the medlar polysaccharide aqueous solution to the medlar seed oil of 1: weighing the wolfberry polysaccharide obtained in the step S41 and the wolfberry seed oil obtained in the step S3 according to the proportion of 0.8-1.2, and adding the weighed wolfberry polysaccharide and wolfberry seed oil into a mixing and stirring device;
s43, adding sorbitan monooleate accounting for 3% -5% of the total mass of the wolfberry polysaccharide aqueous solution and the wolfberry seed oil while performing the step S42; starting a mixing and stirring device to mix and stir the lycium barbarum polysaccharide and the lycium barbarum seed oil to obtain soft capsule contents;
s44, weighing gelatin, adding water, stirring until the gelatin is dissolved, adding glycerol and a light screening agent, and stirring uniformly to obtain a soft capsule shell material;
s45, carrying out capsule pressing treatment on the soft capsule content material obtained in the step S43 and the soft capsule shell material obtained in the step S44 on pressing equipment to obtain the lycium barbarum polysaccharide-lycium barbarum seed oil soft capsule.
2. The method for preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule according to claim 1, which is characterized in that: the viscosity of the medlar polysaccharide with acetyl groups obtained in the step S22 after being prepared into 50% medlar polysaccharide water solution with mass fraction is 450-500 mPa.s, and the viscosity of the medlar polysaccharide with acetyl groups and carboxymethyl groups obtained in the step S23 after being prepared into 50% medlar polysaccharide water solution with mass fraction is 400-450 mPa.s.
3. The method for preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule according to claim 1, which is characterized in that: the viscosity of the soft capsule content obtained in the step S43 is 550 mPas to 600 mPas.
4. The method for preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule according to claim 1, which is characterized in that: the ceramic film in the step S12 is a ceramic film with a 50nm film core.
5. The method for preparing the wolfberry polysaccharide-wolfberry seed oil soft capsule according to claim 1, which is characterized in that: the ultrafiltration membrane in the step S13 is an ultrafiltration membrane with a molecular weight cutoff of 1000-10000 daltons.
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