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CN-122012172-A - Preparation method and application of mussel oil

CN122012172ACN 122012172 ACN122012172 ACN 122012172ACN-122012172-A

Abstract

The invention relates to the technical field of marine biological grease preparation, in particular to a preparation method and application of mussel oil. The invention discloses a preparation method of mussel oil, which comprises the steps of firstly pretreating mussel to obtain homogenate, adding magnetic compound enzyme for enzymolysis, extracting, purifying and aminating to obtain aminated mussel oil, emulsifying the mussel oil, assembling the mussel oil, chitosan and hyaluronic acid layer by layer through electrostatic interaction to form a multi-layer wrapper, adding calcium chloride and sodium alginate for crosslinking, ultrafiltering, sterilizing and filtering to obtain electric field sensitive gel. The method remarkably improves the stability of the mussel oil in the mask through an innovative process of wrapping the multi-layer film and crosslinking the gel, effectively prolongs the quality guarantee period of the mask, and provides a reliable technical path for the development of high-quality mussel oil-related products in the cosmetic field.

Inventors

  • LIU TIANJIAO
  • LIU YONGPING
  • LIU LU

Assignees

  • 广州博士派生物科技有限公司

Dates

Publication Date
20260512
Application Date
20260304

Claims (6)

  1. 1. A preparation method of mussel oil is characterized by comprising the following steps: S001, adding magnetic compound enzyme into mussel homogenate, regulating pH, carrying out enzymolysis, separating by a magnet, and collecting a solution to obtain mussel enzymolysis liquid; S002, adding an extracting agent into the mussel enzymolysis liquid for extraction treatment, and combining extracted organic phases; S003, introducing nitrogen, performing rotary evaporation, and adding rosemary extract to obtain crude mussel oil; S004, heating crude mussel oil, adding ultrapure water, stirring, standing for layering, collecting supernatant, adding sodium hydroxide solution for neutralization, and adding ultrapure water for washing to neutrality; S005, adding activated clay, stirring, filtering, vacuum distilling, and filtering to obtain refined mussel oil; S006, adding the perna canaliculus oil and ethanolamine into a three-neck flask, introducing nitrogen, heating, stirring until the perna canaliculus oil and the ethanolamine are dissolved, adding cyclohexyl carbodiimide and 4-dimethylaminopyridine, adding ethyl acetate for extraction treatment after reaction, combining organic phases, washing and distilling under reduced pressure to obtain the aminated mussel oil, and marking the aminated mussel oil as the mussel oil.
  2. 2. The preparation method of mussel oil according to claim 1, wherein the mussel oil is wrapped by a hyaluronic acid-chitosan multilayer film, the layer-by-layer assembly is realized by utilizing the electrostatic interaction of the hyaluronic acid-chitosan multilayer film and the mussel oil, and the wrapping efficiency of oil-soluble components and the release performance during iontophoresis are simultaneously considered, so that the gel mask containing the mussel oil is obtained, and the preparation method specifically comprises the following steps: s101, mixing mussel oil with tween-80, diluting with phosphate buffer solution, and performing ultrasonic emulsification to obtain mussel oil emulsion; s102, slowly adding an equal volume of chitosan solution, mixing, stirring, centrifuging, discarding the supernatant, and washing for 2 times by using phosphate buffer solution; s103, adding an equal volume of hyaluronic acid solution, stirring, centrifuging, discarding the supernatant, and washing with phosphate buffer solution for 2 times; s104, slowly adding an equal volume of chitosan solution, mixing, stirring, centrifuging, discarding the supernatant, and washing with phosphate buffer solution for 2 times to obtain chitosan-hyaluronic acid-chitosan coated mussel oil, which is marked as a multi-layer wrapper; s105, adding a calcium chloride solution, stirring, adding an equal volume of sodium alginate solution, dropwise adding the calcium chloride solution for crosslinking, ultrafiltering, sterilizing and filtering to obtain the gel mask containing mussel oil.
  3. 3. The method for preparing mussel oil according to claim 1, wherein the mussel homogenate is prepared by washing, desalting, crushing and homogenizing, and comprises the following steps: s201, washing fresh mussel meat, draining, soaking in sodium chloride solution, and rinsing to obtain clean mussel meat; s202, adding clean mussel meat into phosphate buffer solution containing antioxidant, and homogenizing to obtain mussel homogenate.
  4. 4. The preparation method of mussel oil according to claim 1, wherein the magnetic complex enzyme is prepared by a coprecipitation method, magnetic ferroferric oxide nano particles are silanized and glutaraldehyde activated, neutral protease and lipase are immobilized on the surface of a magnetic carrier by utilizing a covalent bond, and the complex enzyme consists of the neutral protease and the lipase, wherein the mass ratio of the complex enzyme to the lipase is 2:1.
  5. 5. The method of preparing mussel oil according to claim 1, wherein the extractant comprises n-hexane and ethanol containing antioxidant at a volume ratio of 3:1, and the antioxidant comprises 0.1% vitamin E and 0.05% citric acid.
  6. 6. The method of claim 3, wherein in step S202, a phosphate buffer solution containing an antioxidant is added according to a feed liquid ratio of 1:2, wherein the antioxidant consists of ethylenediamine tetraacetic acid and tea polyphenol, and the concentrations of the ethylenediamine tetraacetic acid and the tea polyphenol are 0.05%.

Description

Preparation method and application of mussel oil Technical Field The invention relates to the technical field of marine biological grease preparation, in particular to a preparation method and application of mussel oil. Background Marine biological resources have great development potential in the fields of medicine, cosmetics and the like due to unique nutritional ingredients and bioactive substances. Mussels are used as economic shellfish with high yield and wide distribution, are rich in polyunsaturated fatty acids, proteins, vitamins, minerals and other nutritional ingredients, especially omega-3 long-chain polyunsaturated fatty acids, and in-vivo grease is an important source for extracting high-quality marine biological oil. The oil is effectively extracted and utilized in a high-valued way, so that the added value of marine biological resources is obviously improved. Chinese patent publication No. CN116875368A discloses a preparation method of mussel oil, which comprises the steps of mixing mussel meat crushed material with ethanol solution of potassium hydroxide, saponifying, filtering to remove residues, extracting, acidifying, re-extracting and concentrating in vacuum to obtain alkali-extracted mussel oil. Although the alkaline extraction process employed is less costly than supercritical extraction, it requires multiple extraction and acidification operations compared to alcohol extraction, and the alkaline conditions of the alcoholic solution of potassium hydroxide therein may destroy some of the heat sensitive components. Mussel oil is rich in omega-3 long chain polyunsaturated fatty acids, whose unsaturated double bonds are susceptible to oxidation by oxygen, light and temperature, resulting in increased acid number, poor flavor, and no mention of antioxidant strategies, and if exposed to air during vacuum concentration, lipid oxidation may be accelerated. The Chinese patent publication No. CN110100907A discloses a preparation method of a mussel lipid microencapsulation product, which comprises the steps of firstly, extracting grease from mussel freeze-dried powder serving as a raw material by a supercritical carbon dioxide extraction method, secondly, dissolving beta-cyclodextrin and soluble starch in hot water according to a proportion to prepare a wall material solution, then adding soybean lecithin and Tween-80 into the wall material solution, uniformly mixing, then, adding grease according to a certain proportion, stirring and homogenizing to obtain emulsion, carrying out high-pressure homogenization on the emulsion for multiple times, and finally, carrying out spray drying to obtain the microencapsulated powder product. Although the supercritical extraction method can retain more polyunsaturated fatty acids, the strong diffusivity of carbon dioxide during the extraction process may lead to loss of part of the small molecular fatty acids. Supercritical extraction can avoid organic solvent residues, but cannot completely remove heavy metals or algae metabolites in mussel lipids. And the heavy metal removal process is not mentioned in the patent, if the raw material mussel grows in the polluted sea area, the product safety risk can be caused. The wall material adopts beta-cyclodextrin and soluble starch, and can form an embedded structure, but the beta-cyclodextrin and the soluble starch have no antioxidant activity. When the microcapsule wall material is broken, the internal grease lacks oxidation protection. The Chinese patent with publication number CN1304988A discloses a preparation method of three mussel oils, namely firstly, extracting mussel meat by alkaline water decoction, secondly, extracting by acetone reflux, thirdly, extracting by supercritical carbon dioxide extraction under specific pressure, temperature and time. Wherein, the alkaline water is adopted for decoction, and in the process of decoction, the alkaline environment and the high temperature can lead to the saponification reaction of unsaturated fatty acid, thereby damaging the structural integrity of the unsaturated fatty acid. With the acetone reflow method, multiple reflows may lead to degradation of the heat sensitive components. By adopting the supercritical carbon dioxide extraction method, the extraction time is long, the energy consumption cost is increased, and the polar components in the grease can be lost due to long-time carbon dioxide contact. In addition, in the field of cosmetic masks, mussel oil is widely applied because of being rich in active ingredients, but in the mask prepared by the prior art, the mussel oil often faces key problems, on one hand, the mussel oil lacks a high-efficiency wrapping and stabilizing system, is easy to directly contact with air and moisture, and unsaturated double bonds of the mussel oil are rapidly oxidized to cause the active ingredients to lose efficacy, on the other hand, the traditional mask matrix cannot realize the controllable release of the mussel oil, and the ac