CN111548862A - Self-aggregating aqueous phospholipid - Google Patents
Self-aggregating aqueous phospholipid Download PDFInfo
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- CN111548862A CN111548862A CN202010455248.2A CN202010455248A CN111548862A CN 111548862 A CN111548862 A CN 111548862A CN 202010455248 A CN202010455248 A CN 202010455248A CN 111548862 A CN111548862 A CN 111548862A
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- 150000003904 phospholipids Chemical class 0.000 title claims abstract description 340
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 169
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 154
- 239000012530 fluid Substances 0.000 claims abstract description 15
- 239000003921 oil Substances 0.000 claims description 91
- 235000019198 oils Nutrition 0.000 claims description 91
- 238000002791 soaking Methods 0.000 claims description 66
- 235000012424 soybean oil Nutrition 0.000 claims description 65
- 239000003549 soybean oil Substances 0.000 claims description 65
- 229920006395 saturated elastomer Polymers 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 14
- 235000002639 sodium chloride Nutrition 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 11
- 239000011780 sodium chloride Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 235000015165 citric acid Nutrition 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 5
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229960004106 citric acid Drugs 0.000 claims description 2
- 239000003925 fat Substances 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 229940116298 l- malic acid Drugs 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- HWPKGOGLCKPRLZ-UHFFFAOYSA-M monosodium citrate Chemical compound [Na+].OC(=O)CC(O)(C([O-])=O)CC(O)=O HWPKGOGLCKPRLZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000018342 monosodium citrate Nutrition 0.000 claims description 2
- 239000002524 monosodium citrate Substances 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 239000001508 potassium citrate Substances 0.000 claims description 2
- 229960002635 potassium citrate Drugs 0.000 claims description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 2
- 235000011082 potassium citrates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- PHZLMBHDXVLRIX-UHFFFAOYSA-M potassium lactate Chemical compound [K+].CC(O)C([O-])=O PHZLMBHDXVLRIX-UHFFFAOYSA-M 0.000 claims description 2
- 239000001521 potassium lactate Substances 0.000 claims description 2
- 235000011085 potassium lactate Nutrition 0.000 claims description 2
- 229960001304 potassium lactate Drugs 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 229960001790 sodium citrate Drugs 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- 235000012207 sodium gluconate Nutrition 0.000 claims description 2
- 239000000176 sodium gluconate Substances 0.000 claims description 2
- 229940005574 sodium gluconate Drugs 0.000 claims description 2
- 239000001394 sodium malate Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims 2
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims 1
- 229910000027 potassium carbonate Inorganic materials 0.000 claims 1
- 235000011181 potassium carbonates Nutrition 0.000 claims 1
- 239000001540 sodium lactate Substances 0.000 claims 1
- 235000011088 sodium lactate Nutrition 0.000 claims 1
- 229940005581 sodium lactate Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 74
- 230000036571 hydration Effects 0.000 abstract description 27
- 238000006703 hydration reaction Methods 0.000 abstract description 27
- 239000000126 substance Substances 0.000 abstract description 26
- 238000004220 aggregation Methods 0.000 abstract description 25
- 239000002904 solvent Substances 0.000 abstract description 21
- 230000001953 sensory effect Effects 0.000 abstract description 20
- 235000013305 food Nutrition 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000012545 processing Methods 0.000 abstract description 8
- 238000004061 bleaching Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000004519 grease Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 38
- 239000000843 powder Substances 0.000 description 35
- 229920001971 elastomer Polymers 0.000 description 28
- 239000000806 elastomer Substances 0.000 description 28
- 238000001035 drying Methods 0.000 description 22
- 239000004973 liquid crystal related substance Substances 0.000 description 19
- 230000008569 process Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 239000003651 drinking water Substances 0.000 description 12
- 235000020188 drinking water Nutrition 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 11
- 238000004062 sedimentation Methods 0.000 description 11
- 235000013373 food additive Nutrition 0.000 description 9
- 239000002778 food additive Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 8
- 238000007792 addition Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 238000004945 emulsification Methods 0.000 description 6
- 238000009738 saturating Methods 0.000 description 6
- 238000007873 sieving Methods 0.000 description 6
- 235000010469 Glycine max Nutrition 0.000 description 5
- 244000068988 Glycine max Species 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000008347 soybean phospholipid Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000035622 drinking Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 iron ion content Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
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- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000009928 pasteurization Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/05—Organic compounds containing phosphorus as heteroatom
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/10—Phosphatides, e.g. lecithin
- C07F9/103—Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/10—Phosphatides, e.g. lecithin
- C07F9/106—Adducts, complexes, salts of phosphatides
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Nutrition Science (AREA)
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- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention belongs to the technical field of phospholipid processing, and particularly relates to self-aggregating aqueous phospholipid. The self-aggregation water-containing phospholipid comprises main components of phospholipid, grease and water, wherein the water content is 70-80g/100g, the content of acetone insoluble substances is 92.5-95.5g/100g on a dry basis, and the sensory index is brown semitransparent fluid. The invention solves the defects that the content of acetone insoluble substances of the existing water-containing phospholipid is not high and the industry depends on a solvent method for preparing the powdered phospholipid for a long time, and also solves the technical problem that the powdered phospholipid prepared by a hydration method can not realize industrial production. The self-aggregation aqueous phospholipid is used for preparing hydration-method powdered phospholipid, the content of acetone insoluble substances reaches 92.5-95.5g/100g, the color is natural yellow, bleaching is avoided, no solvent exists, the solvent-method powdered phospholipid can be replaced, environmental pollution and food safety hidden trouble caused by solvent-method powdered phospholipid are avoided, and the production cost of the hydration-method powdered phospholipid is far lower than that of a solvent method.
Description
Technical Field
The invention belongs to the technical field of phospholipid processing, and particularly relates to self-aggregating aqueous phospholipid.
Background
The raw material for processing the phospholipid is soybean oil residue, which is called hydrated oil residue for short, is a byproduct of a hydration degumming process in the soybean oil refining process in the field of oil processing, and is also called hydrated oil residue, wherein the main components comprise 30-45g/100g of phospholipid, 20-30g/100g of soybean oil and 30-50g/100g of water, and the trace components comprise metal ions, such as calcium, magnesium, iron and the like, and exist in the form of phospholipid metal salts, such as iron ion content, usually 50-100mg/kg calculated by acetone insoluble substances, and the content is up to more than 150mg/kg in individual cases.
The method for processing the industrial phospholipid mainly comprises two methods, one is that the concentrated phospholipid is prepared by a hydration method, namely the concentrated phospholipid is obtained by directly drying and dehydrating after soybean oil residue is extracted from crude soybean oil in a hydration manner, and the concentrated phospholipid is also called as fluid phospholipid due to the fluidity, and the content of dry acetone insoluble substances is 60-65g/100 g; and secondly, preparing the powdered phospholipid by a solvent method, namely taking soybean oil residue or concentrated phospholipid as a raw material, and extracting the raw material by using acetone to remove grease to obtain the powdered phospholipid, wherein the content of dry acetone insoluble substances is 95-98g/100 g. The mainstream product in the market is concentrated phospholipid, and the ratio of the powdered phospholipid in the market is less than 5%.
Although the soybean oil residue is mostly processed into concentrated phospholipids, the concentrated phospholipids have a great disadvantage. For example, documents "a process for producing concentrated phospholipids from soybean (Huxing. a process for producing concentrated phospholipids from soybean [ J ]. China fat, 2007,32(9):20-21) and" a process for preparing concentrated phospholipids (Houqing et al. a process for preparing concentrated phospholipids [ J ]. China fat, 2002,27(1):39-40) describe a method for producing concentrated phospholipids by dehydrating and oxidizing and bleaching hydrated oil residues as raw materials. The process has the disadvantages that the content of acetone insoluble substances in the concentrated phospholipid is too low (60-65g/100g), chemical bleaching is needed, the market price is only 0.4 ten thousand yuan/ton, and the price has a large difference with the price of 4 ten thousand yuan/ton of powder phospholipid.
Chinese patent CN103665029A discloses a method for preparing soybean powder phospholipid, which adopts acetone as solvent to extract hydrated oil residue, separates out acetone insoluble substances, and then carries out low-temperature vacuum drying on the acetone insoluble substances to remove the solvent, thus obtaining the powder phospholipid. The method has the defects that an acetone solvent is used, the production cost is high, the potential safety hazard of environmental pollution and solvent residue exists, and the method is difficult to popularize generally, so that the structure upgrade of a product converted from concentrated phospholipid to powdered phospholipid in the field of oil processing cannot be promoted, and the current situation of high oil refining loss cannot be improved.
For example, chinese patent CN107325125A discloses a method for preparing a phospholipid hydrate from soybean oil residue and a phospholipid hydrate (hereinafter referred to as phospholipid hydrate) prepared by the method, and the method includes the following steps: adding softened water into soybean oil residue, mixing, standing, and performing chromatography; after the chromatography is finished, controlling the temperature to be 85-95 ℃, and carrying out centrifugal separation to obtain the hydrated phospholipid, wherein the acetone insoluble matter can reach 90-92%. This patent has the following drawbacks:
(1) the dry acetone insoluble content of the hydrated phospholipids is low: the patent is a homogeneous hydration method, namely oil residue and water are mixed uniformly, emulsification inevitably occurs when the mixing is uniform, and phospholipid and oil are difficult to re-separate if the emulsification is serious. In order to avoid serious emulsification, the patent adopts two measures, namely strictly controlling the water adding amount which is 0.25-0.74 times of the weight of oil residue; second, sodium hydroxide or sulfuric acid is added, acting as a demulsifier. The problem brought by the measures is that the main components of phospholipid, grease and phospholipid metal salt in the soybean oil residue are not effectively separated, the content of dry acetone insoluble substances of the hydrated phospholipid reaches only 92 percent at most, and has a certain difference compared with 95-98 percent of acetone insoluble substances in a solvent method;
(2) hydrated phospholipids are not thoroughly dried and lack industrial utility: the hydrated phospholipid is subjected to concentration dehydration, preservative addition, pasteurization and packaging to obtain an aqueous phospholipid product with the water content of 22.5-41.2 percent, but the aqueous phospholipid product does not meet the regulation of national standard GB28401 food additive phospholipid on that the water content cannot exceed 2 percent and cannot be sold; if the drying is performed according to the existing method for preparing powdered phospholipids, the time is too long, the productivity is too low, and the industrial production is not feasible, and the powdered phospholipids can not be sold or further processed, so that the powdered phospholipids are not industrially used.
Another prior art for extracting phospholipid by hydration method is disclosed in the document "research on liquid crystal separation and purification of soybean phospholipid" (Leziming et al. research on liquid crystal separation and purification of soybean phospholipid [ J ]. Chinese food and oil institute, 2007,22(1):31-32), hereinafter referred to as liquid crystal phospholipid. The method of the document has the following technical defects: (1) the content of insoluble acetone on dry basis of the liquid crystal state phospholipid is low: the homogeneous hydration method is adopted, the water adding amount is 0.67 times of oil residue, and the content of the obtained liquid crystal state phospholipid in dry acetone insoluble matters is only 86.05 percent, which is the same as the defect of the hydrated phospholipid; (2) lack of industrial use: the drying problem of the liquid crystal phospholipid is the same as that of the hydrated phospholipid, although the liquid crystal phospholipid is obtained into powder phospholipid by a batch vacuum drying mode, the drying time is too long, and the color of the phospholipid product is dark (brown), so that the liquid crystal phospholipid cannot be applied to industrial production.
Chinese patent CN102517148A discloses a two-step decolorization method of phospholipid, which adopts two-step decolorization methods of hydrogen peroxide bleaching and silica gel adsorption, and has the following defects: (1) chemical bleaching and decoloring, so that phospholipid generates oxidation byproducts, the naturalness of the phospholipid is damaged, and meanwhile, food safety risks exist and the method does not conform to the large trend of green development; (2) the adsorption and decoloration effects of silica gel are poor, and the invalid silica gel becomes waste residue, which is not beneficial to environmental protection; (3) bleaching destroys the beneficial antioxidant components in the phospholipid, reduces the antioxidant and nutritive values of the phospholipid, and shortens the shelf life of the phospholipid.
In the phospholipid processing field, the substitution of the powdered phospholipid for the concentrated phospholipid is the future direction from the product perspective, the substitution of the hydration method for the solvent method is the future direction from the method perspective, and although some researches on the hydration method exist at present, the purity of the phospholipid prepared by the hydration method is not high enough, the color improvement is not separated from the chemical bleaching method, the dehydration efficiency of the hydration method does not reach the industrial level, and the process technology is not enough in the aspects of integrity and continuity.
Therefore, it is necessary to develop a self-aggregating aqueous phospholipid which can solve the above-mentioned technical problems.
Disclosure of Invention
The first object of the present invention is to provide a self-aggregating aqueous phospholipid which has the following advantages: the water content is saturated, the dry acetone insoluble content is the highest in all known hydration methods, and the dry acetone insoluble content is close to or even reaches the level of solvent method powder phospholipid. The self-aggregation aqueous phospholipid is an intermediate product necessary for preparing hydration-method powdered phospholipid, and from the industrial development perspective, the hydration-method powdered phospholipid finally replaces solvent-method powdered phospholipid to become a mainstream product so as to eliminate environmental pollution caused by organic solvent and hidden food safety hazards caused by solvent residue and reduce production cost. The invention solves the technical problem that the prior art can not prepare high-purity water-containing phospholipid and powder phospholipid from soybean oil residue by a hydration method. The self-aggregating aqueous phospholipids have not been reported in the field of phospholipid processing and related studies.
The second object of the present invention is to provide the use of said self-aggregating aqueous phospholipids for the preparation of powdered phospholipids.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a self-aggregating aqueous phospholipid whose main components are phospholipid, oil and fat and water, has a water content of 70-80g/100g and an acetone-insoluble content of 92.5-95.5g/100g on a dry basis.
Preferably, the self-aggregating aqueous phospholipid is a brown translucent fluid.
The self-aggregation water-containing phospholipid refers to an aggregate formed by the spontaneous combination and the spontaneous aggregation of phospholipid in the soybean oil residue and water.
Preferably, the method for preparing the self-aggregating aqueous phospholipid comprises the following steps: soaking soybean oil residue in water to obtain saturated water-absorbing oil residue, and naturally settling.
The soaking means that the soybean oil residue is a dispersed phase in water, and the water is a continuous phase, so that a soaking system is formed.
As a result of the soaking, a saturated water-absorbing oil foot was obtained. And after soaking, the water absorption capacity of the phospholipid in the saturated water absorption oil residue reaches saturation, namely the water content of the phospholipid reaches 70-80g/100 g.
More preferably, the mass ratio of the soybean oil foot to the water is 1: 1-3.5.
When the weight of the water is less than 1.0 time of that of the oil residue, the soybean oil residue can not be effectively soaked in the water, and the combination of the phospholipid and the water is further influenced. When the water is more than 3.5 times of the mass of the oil residue, although the soaking of the soybean oil residue is facilitated, the cost of water, the energy consumption and the volume of the equipment are increased.
More preferably, the temperature of the soaking is 60-95 ℃.
In water at 0 ℃ to 100 ℃, the combination of phospholipid and water can occur, and the combination efficiency is higher at higher temperature. Therefore, the water temperature is increased, and the soaking time can be shortened. However, in boiling water, stabilization of self-aggregating aqueous phospholipids is not favored, and boiling evaporation of water wastes energy. The temperature of the soaking is therefore preferably 60-95 ℃. When the temperature is above 60 deg.C, the sterilization temperature can prevent oil residue from deteriorating during soaking, and when the temperature is below 95 deg.C, water can be prevented from boiling.
More preferably, the soaking time is 1-3 h.
The soaking time refers to the time required for obtaining the saturated water-absorbing oil foot, and the soaking time is from the time when the soybean oil foot is in a granular shape and stands still in water for soaking until brown self-aggregation water-containing phospholipid begins to appear in the soybean oil foot. The soybean oil residue in the soaking was yellow and the self-aggregating aqueous phospholipid appeared brown, so that it was possible to visually judge whether the end time of the soaking was reached.
More preferably, the soaking is still soaking.
During the soaking period, stirring operation is not suitable to prevent emulsification.
More preferably, the soybean oil foot is broken up into particles in water with stirring before soaking.
More preferably, the particle size of the soybean oil foot particles is less than or equal to 5 mm.
More preferably, the particle size of the soybean oil foot particles is 0.3 to 3 mm.
The smaller the particle size of the soybean oil residue is, the larger the contact area of the oil residue and water is, and the mass transfer and heat transfer efficiency of phospholipid and water in the soybean oil residue is improved. However, the soybean oil residue has a too small particle size, and there is a risk that the soybean oil residue and water are uniformly mixed and homogenized, and the soaking system is damaged.
More preferably, the preparation method further comprises adding an electrolyte to the soaking system.
More preferably, the electrolyte has a mass fraction in water of 0.01 to 0.3%.
The proper amount of electrolyte is beneficial to the combination of the phospholipid and water in the soybean oil residue, the combination of the phospholipid and the water can be inhibited when the electrolyte is too much, and the water content of the self-aggregation water-containing phospholipid is higher when the electrolyte is too little or not added, so that the energy waste during dehydration is caused.
More preferably, the electrolyte includes at least one of an acid, a base, and a salt.
More preferably, the electrolyte is at least one of DL-sodium malate, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, monosodium citrate, sodium gluconate, lactic acid, potassium lactate, sodium carbonate, potassium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid, and sodium chloride.
More preferably, the time of natural settling is 3-8 h.
As a result of said natural sedimentation, self-aggregating aqueous phospholipids are obtained. At the end of natural sedimentation, two components, namely the self-aggregating aqueous phospholipid and the residue of the oil residue, are obtained from the saturated water-absorbing oil residue. During the natural settling period, stirring operation is not suitable to prevent emulsification.
The invention also relates to the use of said self-aggregating aqueous phospholipids for preparing powdered phospholipids.
Preferably, the self-aggregating aqueous phospholipid is used for preparing a powdered phospholipid, comprising the steps of:
(1) preparation of concentrated aqueous phospholipids: concentrating the self-aggregating aqueous phospholipid under vacuum at 90-110 deg.C to a water content of 25-65g/100g to obtain a concentrated aqueous phospholipid having a dry acetone insoluble content of 92.5-95.5g/100g and a sensory index of brown translucent fluid.
(2) Preparation of aqueous phospholipid elastomer: and pushing the concentrated aqueous phospholipid into a stirrer at the speed of 10-100cm/min, wherein the stirring rotation number is 800-1200rpm, and the stirring time is 5-30s, so as to obtain the continuously output aqueous phospholipid elastomer, wherein the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index is changed into yellow opaque semisolid.
The aqueous phospholipid elastomer is an elastomer in the colloid chemistry category, the rheological property of the aqueous phospholipid elastomer is that the storage modulus G 'is 5-10 times larger than the loss modulus G' and the aqueous phospholipid elastomer shows stronger solid characteristics (elasticity) and weaker liquid characteristics (viscosity) and belongs to the elastomer.
(3) Preparing solid phospholipid: and (2) feeding the continuously output water-containing phospholipid elastomer into a normal-pressure or vacuum continuous dryer through a feed inlet with the aperture of 2-6mm, and drying at the temperature of 120-160 ℃ for 6-20min to obtain continuously output strip-shaped solid phospholipid, wherein the water content of the strip-shaped solid phospholipid is 3-10g/100g, the content of the dry acetone insoluble substances is 92.5-95.5g/100g, and the sensory index of the strip-shaped solid is yellow strip-shaped solid.
(4) Preparing powder phospholipid: and (2) crushing and sieving the strip-shaped solid phospholipid, and performing vacuum drying at 60 ℃ for 30-60min to obtain powder phospholipid, wherein the water content of the powder phospholipid is less than or equal to 2g/100g, the content of dry acetone insoluble substances is 92.5-95.5g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.
The water content of the powder phospholipid in the step (4) is equal to the drying decrement described in the national standard GB28401 food additive phospholipid.
The vacuum is 0.01-0.004 MPa.
The invention has the beneficial effects that:
firstly, the water content of the self-aggregation water-containing phospholipid reaches 70-80g/100g, the water absorption capacity of the phospholipid reaches saturation: when the water absorption capacity of the phospholipid reaches saturation, the lipophilicity of the phospholipid is reduced to the minimum, namely the oil content of the self-aggregation water-containing phospholipid is the minimum, the purity of the phospholipid is the highest, and the content of dry acetone insoluble matters reaches 92.5-95.5g/100 g.
Second, the dry acetone insoluble content of the self-aggregating aqueous phospholipids of the present invention is highest in all current hydration processes: the dry acetone insoluble content of the self-aggregation water-containing phospholipid is 92.5-95.5g/100g, the content of the patent-disclosed hydrated phospholipid is 90-92g/100g, and the content of the liquid crystal state phospholipid reported in the literature is 86.05g/100 g.
Third, the dry acetone insoluble content of the self-aggregating aqueous phospholipids of the present invention is most similar to the solvent method: the dry acetone insoluble content of the self-aggregating aqueous phospholipid of the invention is 92.5-95.5g/100g, which is close to or even reaches the level of 95-98g/100g of solvent method powder phospholipid. From the perspective of industrial development, a hydration method is a mainstream product to replace a solvent method finally so as to eliminate environmental pollution caused by organic solvent and food safety hidden trouble caused by solvent residue and reduce production cost.
Fourthly, the self-aggregation aqueous phospholipid and the powder phospholipid prepared by the self-aggregation aqueous phospholipid have complete process technology from soybean oil residue to powder phospholipid, have great advantages in the aspects of quality, quality guarantee period, production cost, environmental protection and food safety, and are suitable for industrial production.
Drawings
FIG. 1 is a process flow diagram of a process for obtaining self-aggregating aqueous phospholipids by soaking soybean oil foot and naturally settling.
FIG. 2 is a schematic diagram of a process for obtaining self-aggregating aqueous phospholipids by soaking soybean oil bottoms and naturally settling. Wherein:
(a) is a schematic diagram of soybean oil foot in water;
(b) the soaking system is a schematic diagram of a soaking system with soybean oil residue particles as a dispersed phase and water as a continuous phase;
(c) a schematic diagram of self-aggregating aqueous phospholipids with natural sedimentation beginning with saturated water-absorbing oil bottoms;
(d) is a schematic diagram of the saturated water-absorbing oil residue which is naturally settled to obtain the self-aggregating aqueous phospholipid and the oil residue.
FIG. 3 is a process flow diagram for preparing solid phospholipids from aggregated aqueous phospholipids.
FIG. 4 is a schematic diagram of a process for concentrating aqueous phospholipids to prepare solid phospholipids.
FIG. 5 is a graph of the rheological characteristics of storage modulus G 'and loss modulus G' for aqueous phospholipid elastomers prepared using the self-aggregating aqueous phospholipid of example 1.
FIG. 6 is a graph showing the rheological characteristics of storage modulus G 'and loss modulus G' of an aqueous phospholipid elastomer prepared by self-aggregating an aqueous phospholipid in application example 2.
Wherein: (1) is a continuous phase of water; (2) is soybean oil residue; (3) is dispersed phase soybean oil foot particles; (4) is saturated water absorption oil residue; (5) is a self-aggregating aqueous phospholipid; (6) is residue of oil residue; (7) is a concentrated aqueous phospholipid; (8) is an aqueous phospholipid elastomer; (9) is a solid phospholipid. A is a soaking tank; b is a speed-regulating gear pump; c is a pipeline stirrer; d is a continuous dryer.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are commercially available; the vacuum is 0.01-0.004 MPa.
Definition of dry acetone insoluble yield from aggregated aqueous phospholipids:
the yield of dry acetone insoluble matter of self-aggregated aqueous phospholipid is the weight of dry acetone insoluble matter of self-aggregated aqueous phospholipid/the weight of dry acetone insoluble matter of soybean oil residue.
Example 1
A self-aggregating aqueous phospholipid is prepared by referring to FIG. 1 and FIGS. 2(a) -2 (d), and the preparation method comprises the following steps:
(1) soaking: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 60 ℃, and the soaking time is 3h to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The soybean oil residue is from Zhongliangyouyue (Tianjin) Co., Ltd, and the material composition is as follows: the water content was 41.03g/100g, the content of acetone insolubles on a dry basis was 61.13g/100 g; the water is drinking water; the mass ratio of oil residue to water is 1: 1; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 3h to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 77.78g/100g, a dry acetone insoluble content of 93.81g/100g, a brown translucent fluid as sensory index, and a yield of 75.63% dry acetone insoluble of the self-aggregated aqueous phospholipid.
Example 2
A self-aggregating aqueous phospholipid is prepared by referring to FIG. 1 and FIGS. 2(a) -2 (d), and the preparation method comprises the following steps:
(1) soaking: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 70 deg.C, and the soaking time is 3 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The oil residue is from the food and grain industry (Jiujiang) limited company, and the material composition of the oil residue is as follows: the water content was 37.56g/100g, the dry acetone insoluble content was 60.87g/100 g; the water is purified drinking water, salt and sodium chloride are added into the water, and the adding amount of the salt and the sodium chloride is 0.07 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 1.5; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural sedimentation for 8h to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 74.00g/100g, a dry acetone insoluble content of 93.75g/100g, a brown translucent fluid as sensory index, and a yield of 78.09% of dry acetone insoluble matter.
Example 3
A self-aggregating aqueous phospholipid, as shown in FIG. 1 and FIGS. 2(a) to 2(d), which is prepared by a method comprising the steps of:
(1) soaking: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 80 deg.C, and the soaking time is 2 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The oil residue is from the food, grain and oil industry (Huanggang) Co., Ltd, and the material composition is as follows: the water content is 38.42g/100g, and the content of acetone insoluble matter is 61.02g/100 g; the water is purified drinking water, food additive lactic acid with the concentration of 80% is added into the water, and the adding amount is 0.05% of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 2; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 4 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 73.12g/100g, a dry acetone insoluble content of 92.53g/100g, a sensory index of brown translucent fluid, and a yield of dry acetone insoluble of the self-aggregated aqueous phospholipid of 80.72%.
Example 4
A self-aggregating aqueous phospholipid, as shown in FIG. 1 and FIGS. 2(a) to 2(d), which is prepared by a method comprising the steps of:
(1) soaking: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 90 deg.C, and the soaking time is 2 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The oil foot is from the Pongji (Nanjing) grain and oil Co., Ltd, and the material composition of the oil foot is as follows: the water content is 39.78g/100g, and the content of acetone insoluble matter is 62.05g/100 g; the water is purified drinking water, and a food additive sodium hydroxide is added into the water, wherein the addition amount of the sodium hydroxide is 0.03 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 2.5; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 5h to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 77.56g/100g, a dry acetone insoluble content of 95.42g/100g, a brown translucent fluid as sensory index, and a dry acetone insoluble yield of 82.71%.
Example 5
A self-aggregating aqueous phospholipid, as shown in FIG. 1 and FIGS. 2(a) to 2(d), which is prepared by a method comprising the steps of:
(1) soaking: adding soybean oil residue into water, and stirring to break the oil residue into granules in water to form a soaking system with soybean oil residue granules as disperse phase and water as continuous phase, wherein the soaking temperature is 95 deg.C, and the soaking time is 1 hr to obtain saturated water-absorbing oil residue. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The oil residue is from the grain and oil limited company of Zhongbao Zhenjiang, and the material composition is as follows: the water content was 37.69g/100g, the content of acetone insolubles on a dry basis was 63.45g/100 g; the water is purified drinking water, food additives of citric acid and common salt and sodium chloride are added into the water, the addition amount of the citric acid is 0.028 percent of the weight of the purified drinking water, and the addition amount of the common salt is 0.052 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 3; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural settling for 6 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 72.33g/100g, a dry acetone insoluble content of 93.65g/100g, a brown translucent fluid as sensory index, and a dry acetone insoluble yield of 83.35%.
Example 6
A self-aggregating aqueous phospholipid, as shown in FIG. 1 and FIGS. 2(a) to 2(d), which is prepared by a method comprising the steps of:
(1) soaking: adding soybean oil foot into water, and stirring to break the oil foot into granules in water to form a soaking system with soybean oil foot granules as disperse phase and water as continuous phase, wherein the soaking temperature is 95 ℃, and the soaking time is 1h to obtain saturated water absorption oil foot. The saturated water-absorbing oil foot is marked by the initial appearance of brown self-aggregating aqueous phospholipids.
The oil foot is from China spinning grain oil (Dongguan) Co., Ltd, and the material composition of the oil foot is as follows: the water content was 40.23g/100g, the content of acetone insolubles on a dry basis was 62.39g/100 g; the water is purified drinking water, and a food additive citric acid is added into the water, wherein the addition amount of the citric acid is 0.038 percent of the weight of the purified drinking water; the mass ratio of oil residue to water is 1: 3.5; the grain diameter of the oil residue particles is 0.3-3 mm.
(2) And (3) natural sedimentation: and (3) saturating the water-absorbing oil residue, and keeping the soaking temperature for natural sedimentation for 7 hours to obtain the self-aggregation water-containing phospholipid and the oil residue.
The obtained self-aggregated aqueous phospholipid had a water content of 73.01g/100g, a dry acetone insoluble content of 94.18g/100g, a brown translucent fluid as sensory index, and a yield of dry acetone insoluble of 83.98% of the self-aggregated aqueous phospholipid.
Comparative example 1
A method for preparing hydrated phospholipid from soybean oil foot is disclosed in patent CN107325125A, and comprises the following steps:
adding 0.53 times of drinking purified water and 0.03% of sulfuric acid into soybean oil residue, heating to 85 deg.C, standing for 6 hr, and centrifuging at 85 deg.C and 4500r/min for 5min to obtain hydrated phospholipid. The soybean oil residue is produced by the food and grain and oil industry (Huanggang) Co Ltd, the water content is 38.42g/100g, and the content of dry acetone insoluble matter is 61.02g/100 g.
The resulting hydrated phospholipid had a water content of 64.03g/100g, a dry acetone insoluble content of 90.01g/100g, and a sensory index of brown translucent fluid.
Compared with the hydrated phospholipid prepared in the comparative example 1, the main differences comprise the following aspects:
first, hydration method and phospholipid water content differ: the hydrated phospholipid is prepared by a homogeneous hydration method, soybean oil residue and water need to be uniformly mixed, the water adding amount in the hydration operation is 0.25-0.74 times of the weight of the oil residue, and the water is more than that of the oil residue, so the water absorption capacity of the hydrated phospholipid is far from the saturation degree, and the water content of the phospholipid is only 64.03g/100 g; the self-aggregation water-containing phospholipid is prepared by a soaking hydration method, soybean oil residue takes granules as a disperse phase, water is taken as a continuous phase to form a soaking system, the water adding amount in the hydration operation is 1.0-3.5 times of the weight of the oil residue, so that redundant free water is ensured to exist around the phospholipid, the water absorption capacity of the phospholipid is ensured to be saturated, and the saturation value is 70-80g/100 g. Only when the water content of the phospholipids is saturated, the acetone-insoluble content of the phospholipids reaches a maximum value, which is 92.5-95.5g/100 g.
Secondly, the phospholipid purity was different: the content of dry acetone insoluble matter of the hydrated phospholipid is 90-92g/100 g; the content of the dry acetone insoluble substances of the self-aggregation water-containing phospholipid is 92.5-95.5g/100g, which is the highest content in the phospholipid by the existing hydration method and is close to or even reaches the level of 95-98g/100g by the solvent method.
Comparative example 2
A method for preparing liquid crystal state phospholipid from soybean oil foot is derived from the research on liquid crystal state separation and purification of soybean phospholipid in the literature, and comprises the following steps:
adding 0.67 times of drinking purified water to soybean oil residue, mixing, heating to 70 deg.C, standing for 4 hr, and centrifuging at 70 deg.C and 4500r/min for 5min to obtain liquid crystal phospholipid. The soybean oil foot was produced by Zhongwan grain oil (Dongguan) Co., Ltd., and had a water content of 40.23g/100g and a dry acetone insoluble content of 62.39g/100 g.
The obtained liquid crystalline phospholipid had a water content of 63.89g/100g, a dry acetone insoluble content of 86.23g/100g, and a sensory index of brown translucent fluid.
Liquid crystal state phospholipid is distributed on a drying tray through a group of circular feed inlets with the aperture of 2mm, and is dried for 240min at 65 ℃ in an intermittent vacuum drying oven to obtain brown massive solid phospholipid, the water content of which is 6.38g/100g, and the content of dry acetone insoluble substances is 86.23g/100 g; and (3) crushing the brown solid phospholipid, sieving the crushed brown solid phospholipid by a 18-mesh sieve, and drying the powder phospholipid in a vacuum drying oven at 60 ℃ for 30min to obtain powder phospholipid with the water content of 1.24g/100g, the content of dry acetone insoluble substances of 86.23g/100g and the sensory index of brown powder.
Compared with the liquid crystal state phospholipid prepared in the comparative example 2, the liquid crystal state phospholipid mainly has the following differences:
first, the degree of hydration is different: the water content of the liquid crystal state phospholipid is only 63.89g/100g, the liquid crystal state phospholipid is prepared by a homogeneous hydration method, soybean oil residue and water need to be uniformly mixed, the water addition amount needs to be strictly controlled, otherwise emulsification can occur, and the water addition amount in the hydration operation is 0.67 times of the weight of the oil residue, so the water absorption amount of the liquid crystal state phospholipid is far from the saturation degree, and the defect is completely the same as that of the patent hydrated phospholipid; the water content of the self-aggregation water-containing phospholipid is 70-80g/100g, the self-aggregation water-containing phospholipid is prepared by a soaking hydration method, the soybean oil foot takes a granular shape as a dispersed phase and takes water as a continuous phase to form a soaking system, and the water adding amount in the hydration operation is 1.0-3.5 times of the weight of the oil foot, so that the water absorption capacity of the phospholipid is ensured to be saturated. The acetone insoluble content of phospholipids can only reach a maximum value if the water absorption capacity of the phospholipids is saturated.
Secondly, the phospholipid purity was different: the content of the liquid crystal state phospholipid in the dry acetone insoluble matter is only 86.23g/100g, the solid phospholipid prepared by drying is brown, and the powder phospholipid is brown; the content of the dry acetone insoluble substance of the self-aggregation water-containing phospholipid is 92.5-95.5g/100g, and the content of the dry acetone insoluble substance of the self-aggregation water-containing phospholipid is greatly different from that of the dry acetone insoluble substance of the self-aggregation water-containing phospholipid. Both the solid phospholipid and the powdered phospholipid prepared by self-aggregating aqueous phospholipid are yellow.
Comparative example 3
A method for preparing powdered soybean phospholipid is disclosed in patent CN103665029A, and comprises the following steps:
mixing soybean oil residue and anhydrous acetone in a weight ratio of 1:10, stirring and extracting for 20min under the conditions of normal pressure and room temperature, performing centrifugal separation for solid-liquid separation, wherein the centrifugal time is 1min, the centrifugal speed is 4000rpm, and collecting solid parts.
The soybean oil foot is from the Pongji (Nanjing) grain and oil Co., Ltd, and the material composition of the soybean oil foot is as follows: the water content was 39.78g/100g, and the dry acetone insoluble content was 62.05g/100 g.
Mixing the solid part obtained in the step with anhydrous acetone in a weight ratio of 1:10, stirring and extracting for 20min under the conditions of normal pressure and room temperature, then performing centrifugal separation for solid-liquid separation, wherein the centrifugal speed is 5000rpm, and collecting the solid part, wherein the centrifugal time is 1 min. Crushing the solid part, and drying at 60 deg.C under vacuum for 5 hr to obtain soybean powder phospholipid, wherein the content of insoluble acetone is 95.30g/100g, and the weight loss is 0.65g/100g, and the soybean powder phospholipid is brown powder.
Compared with the powder phospholipid prepared in the comparative example 3, the main differences comprise the following aspects:
first, the difference between environmental protection and food safety: the comparative example 3 is the powdered phospholipid prepared by the solvent method, the solvent method has the environmental pollution caused by solvent volatilization, the drying loss of the product is 0.65g/100g, the components reduced by drying are the solvent, and the potential safety hazard of food with residual solvent exists; the powder phospholipid prepared by the application of the invention belongs to a hydration method, has no environmental pollution, the drying decrement of the product is less than or equal to 2g/100g, the component of the drying decrement is water, and no potential safety hazard of food exists.
Secondly, the differences in color and luster: the powdered phospholipid prepared in comparative example 3 was brown, and the color of the phospholipid was darker in order to reduce the residual solvent and prolong the drying time; the self-aggregating aqueous phospholipid of the invention has short drying time when preparing powder phospholipid, and the color of the phospholipid is natural yellow.
Application example 1
Use of the aqueous phospholipid self-aggregated in example 2 to prepare solid phospholipid, powdered phospholipid, with reference to fig. 3 and 4, comprising the following steps:
(1) concentrating the self-aggregating aqueous phospholipid prepared in example 2 to obtain a concentrated aqueous phospholipid; (2) stirring the concentrated aqueous phospholipid to obtain an aqueous phospholipid elastomer; (3) drying the aqueous phospholipid elastomer to obtain strip-shaped solid phospholipid; (4) and (3) crushing, sieving and drying the strip-shaped solid phospholipid to obtain the powdery phospholipid.
Step (1) preparation of concentrated aqueous phospholipid: the self-aggregating aqueous phospholipid of example 2 was concentrated to a water content of 55g/100g at 95 ℃ in a vacuum thin film evaporator to give a concentrated aqueous phospholipid having a dry acetone insoluble content of 93.75g/100g and an organoleptic index of brown translucent fluid.
Step (2) preparation of aqueous phospholipid elastomer: and (2) pushing the concentrated aqueous phospholipid obtained in the step (1) into a stirrer at the speed of 80cm/min, wherein the stirring speed is 900rpm, and the stirring time is 10s, so that the continuously output aqueous phospholipid elastomer is obtained, and the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index is changed into yellow opaque semisolid.
Preparing solid phospholipid by the step (3): and (3) feeding the water-containing phospholipid elastomer continuously output in the step (2) into a normal-pressure continuous dryer through a group of feed inlets with the aperture of 3mm, and drying at 150 ℃ for 8min to obtain continuously output strip-shaped solid phospholipid, wherein the water content of the strip-shaped solid phospholipid is 7.23g/100g, the content of dry acetone insoluble substances is 93.75g/100g, and sensory indexes of the strip-shaped solid are yellow strip-shaped solids.
Step (4) preparation of powdered phospholipids: and (3) crushing the strip-shaped solid phospholipid obtained in the step (3), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 40min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.43g/100g, the content of the dry acetone insoluble substances is 93.75g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.
Application example 2
Use of the self-aggregating aqueous phospholipids from example 4 to prepare solid phospholipids, powdered phospholipids, with reference to fig. 3 and 4, comprising the following steps:
(1) concentrating the self-aggregating aqueous phospholipid prepared in example 4 to obtain a concentrated aqueous phospholipid; (2) stirring the concentrated aqueous phospholipid to obtain an aqueous phospholipid elastomer; (3) drying the aqueous phospholipid elastomer to obtain strip-shaped solid phospholipid; (4) and (3) crushing, sieving and drying the strip-shaped solid phospholipid to obtain the powdery phospholipid.
Step (1) preparation of concentrated aqueous phospholipid: the self-aggregating aqueous phospholipid of example 4 was concentrated to a water content of 45g/100g at 105 ℃ in a vacuum thin film evaporator to give a concentrated aqueous phospholipid having a dry acetone insoluble content of 95.42g/100g and an organoleptic index of brown translucent fluid.
Step (2) preparation of aqueous phospholipid elastomer: and (2) pushing the concentrated aqueous phospholipid obtained in the step (1) into a stirrer at the speed of 40cm/min, wherein the stirring speed is 1100rpm, and the stirring time is 20s, so that the continuously output aqueous phospholipid elastomer is obtained, and the water content and the acetone insoluble content of the aqueous phospholipid elastomer are the same as those of the concentrated aqueous phospholipid, but the sensory index of the aqueous phospholipid elastomer is changed into yellow opaque semisolid.
Preparing solid phospholipid by the step (3): and (3) feeding the water-containing phospholipid elastomer continuously output in the step (2) into a vacuum continuous dryer through a group of feed inlets with the aperture of 4mm, and drying at 130 ℃ for 15min to obtain continuously output strip-shaped solid phospholipid, wherein the water content of the strip-shaped solid phospholipid is 5.32g/100g, the content of dry acetone insoluble substances is 95.42g/100g, and the sensory index of the strip-shaped solid is yellow strip-shaped solid.
Step (4) preparation of powdered phospholipids: and (3) crushing the strip-shaped solid phospholipid obtained in the step (3), sieving the powder with a 18-mesh sieve, and performing vacuum drying in a double-cone rotary vacuum dryer at 60 ℃ for 30min to obtain powder phospholipid, wherein the water content of the powder phospholipid is 1.18g/100g, the content of the dry acetone insoluble substances is 95.42g/100g, the sensory index of the powder phospholipid is yellow powder, and the product meets the national standard GB28401 food additive phospholipid.
Test example 1
The aqueous phospholipid elastomers prepared in example 1 and application example 2 were rheologically characterized, and the test results are shown in fig. 5 and 6, respectively. The instruments and parameters used for detection are as follows: RS6000 rotational rheometer (HAAKE, Germany), the measuring rotor used a Z41Ti coaxial drum sensing system (drum and rotor diameters 43.40mm and 41.42mm, respectively) with a sample thickness of 3mm in the center of the sensing system.
As can be seen from FIGS. 5 and 6, the aqueous phospholipid elastomers provided in application examples 1 and 2 have storage modulus G 'more than 5 times larger than loss modulus G' in the measured frequency range, and they are almost independent of frequency, indicating that elasticity is much larger than viscosity, showing stronger solid characteristics (elasticity), while liquid characteristics (viscosity) become weaker and belong to elastomers.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. A self-aggregating aqueous phospholipid, characterized in that the main components of the self-aggregating aqueous phospholipid are phospholipid, oil and fat and water, the water content is 70-80g/100g, and the acetone insoluble content is 92.5-95.5g/100g on a dry basis.
2. The self-aggregating aqueous phospholipid as set forth in claim 1, wherein the self-aggregating aqueous phospholipid is a brown translucent fluid.
3. The self-aggregating aqueous phospholipid as set forth in claim 1, wherein the preparation method of the self-aggregating aqueous phospholipid comprises the steps of: soaking soybean oil residue in water to obtain saturated water-absorbing oil residue, and naturally settling.
4. The self-aggregating aqueous phospholipid as claimed in claim 3, wherein the mass ratio of the soybean oil foot to the water is 1:1 to 3.5.
5. The self-aggregating aqueous phospholipid as set forth in claim 3, wherein the soaking temperature is 60 to 95 ℃, the soaking time is 1 to 3 hours, and the natural settling time is 3 to 8 hours.
6. The self-aggregating aqueous phospholipid as claimed in claim 3, wherein the soybean oil foot is broken up in water into granules with a particle size of 5mm or less, preferably 0.3 to 3mm, by stirring before the soaking.
7. The self-aggregating aqueous phospholipid as set forth in claim 3, wherein the preparation method further comprises adding an electrolyte to the soaking system.
8. The self-aggregating aqueous phospholipid as claimed in claim 7, wherein the electrolyte has a mass fraction in water of 0.01 to 0.3%.
9. The self-aggregating aqueous phospholipid of claim 7, wherein the electrolyte comprises at least one of an acid, a base and a salt, preferably the electrolyte is at least one of DL-sodium malate, L-malic acid, DL-malic acid, glacial acetic acid, citric acid, potassium citrate, sodium citrate, monosodium citrate, sodium gluconate, lactic acid, potassium lactate, sodium lactate, potassium carbonate, sodium carbonate, potassium bicarbonate, sodium sulfate, potassium chloride, potassium hydroxide, sodium hydroxide, hydrochloric acid, phosphoric acid and sodium chloride.
10. Use of a self-aggregating aqueous phospholipid as defined in any one of claims 1 to 9 in the preparation of a powdered phospholipid.
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| PCT/CN2020/135902 WO2021238162A1 (en) | 2020-05-26 | 2020-12-11 | Self-aggregating aqueous phospholipid and preparation method therefor |
| US17/830,423 US20220298184A1 (en) | 2020-05-26 | 2022-06-02 | Self-aggregating hydrous phospholipid and preparation method thereof |
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| WO2021238162A1 (en) * | 2020-05-26 | 2021-12-02 | 内蒙古铂贝曼科技有限公司 | Self-aggregating aqueous phospholipid and preparation method therefor |
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