CN115010750B - Soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio and preparation method thereof - Google Patents
Soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio and preparation method thereof Download PDFInfo
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- 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 title claims abstract description 69
- 229940083466 soybean lecithin Drugs 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000004698 Polyethylene Substances 0.000 title abstract description 9
- 239000004417 polycarbonate Substances 0.000 title abstract description 9
- -1 polyethylene Polymers 0.000 title abstract description 7
- 229920000515 polycarbonate Polymers 0.000 title abstract description 5
- 229920000573 polyethylene Polymers 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000605 extraction Methods 0.000 claims abstract description 47
- 239000000284 extract Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000012046 mixed solvent Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 150000003904 phospholipids Chemical class 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 39
- 238000002425 crystallisation Methods 0.000 claims description 21
- 230000008025 crystallization Effects 0.000 claims description 21
- 239000006228 supernatant Substances 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 239000010408 film Substances 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 15
- 239000008347 soybean phospholipid Substances 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000001179 sorption measurement Methods 0.000 claims description 13
- 230000003068 static effect Effects 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 9
- 125000004122 cyclic group Chemical group 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000011082 depyrogenation Methods 0.000 claims 2
- 239000002510 pyrogen Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 9
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 abstract description 5
- 239000000787 lecithin Substances 0.000 abstract description 5
- 229940067606 lecithin Drugs 0.000 abstract description 5
- 235000010445 lecithin Nutrition 0.000 abstract description 5
- 239000003995 emulsifying agent Substances 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 235000013376 functional food Nutrition 0.000 abstract description 2
- 235000016709 nutrition Nutrition 0.000 abstract description 2
- 239000000825 pharmaceutical preparation Substances 0.000 abstract description 2
- 239000012994 photoredox catalyst Substances 0.000 abstract 1
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 42
- JZNWSCPGTDBMEW-UHFFFAOYSA-N Glycerophosphorylethanolamin Natural products NCCOP(O)(=O)OCC(O)CO JZNWSCPGTDBMEW-UHFFFAOYSA-N 0.000 description 39
- 150000008104 phosphatidylethanolamines Chemical class 0.000 description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 31
- 150000003905 phosphatidylinositols Chemical class 0.000 description 16
- 238000004458 analytical method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000004128 high performance liquid chromatography Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000000638 solvent extraction Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000005374 membrane filtration Methods 0.000 description 5
- 238000004440 column chromatography Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 235000010469 Glycine max Nutrition 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- MUPFEKGTMRGPLJ-RMMQSMQOSA-N Raffinose Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](O[C@@]2(CO)[C@H](O)[C@@H](O)[C@@H](CO)O2)O1)[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 MUPFEKGTMRGPLJ-RMMQSMQOSA-N 0.000 description 1
- UQZIYBXSHAGNOE-USOSMYMVSA-N Stachyose Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@H](O)[C@@H](O[C@@]2(CO)[C@H](O)[C@@H](O)[C@@H](CO)O2)O1)[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@H](CO[C@@H]2[C@@H](O)[C@@H](O)[C@@H](O)[C@H](CO)O2)O1 UQZIYBXSHAGNOE-USOSMYMVSA-N 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 208000003441 Transfusion reaction Diseases 0.000 description 1
- MUPFEKGTMRGPLJ-UHFFFAOYSA-N UNPD196149 Natural products OC1C(O)C(CO)OC1(CO)OC1C(O)C(O)C(O)C(COC2C(C(O)C(O)C(CO)O2)O)O1 MUPFEKGTMRGPLJ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- XLSMFKSTNGKWQX-UHFFFAOYSA-N hydroxyacetone Chemical compound CC(=O)CO XLSMFKSTNGKWQX-UHFFFAOYSA-N 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000001990 intravenous administration Methods 0.000 description 1
- 239000002960 lipid emulsion Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- MUPFEKGTMRGPLJ-ZQSKZDJDSA-N raffinose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)O1 MUPFEKGTMRGPLJ-ZQSKZDJDSA-N 0.000 description 1
- UQZIYBXSHAGNOE-XNSRJBNMSA-N stachyose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO[C@@H]3[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O3)O)O2)O)O1 UQZIYBXSHAGNOE-XNSRJBNMSA-N 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
Abstract
The invention discloses a preparation method of soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio, which is characterized in that concentrated soybean lecithin is used as a raw material, an alcohol-water mixed solvent is adopted for extraction and deoiling to obtain deoiled lecithin, the deoiled lecithin is circularly extracted by ethanol to obtain an extract, and the extract is subjected to the procedures of low-temperature freeze separation, heat source removal, vacuum centrifugal film concentration and vacuum low-temperature drying to obtain transparent soybean lecithin with the PC and PE ratio of 3.5-8.0. The solvent used in the method is safe and nontoxic, is easy for industrialized and continuous production, has high productivity, low cost and high total yield and purity, and the prepared product does not contain heat source components, has stable and controllable quality, and the soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio prepared by the method can be widely applied to industries of medicines, health-care foods, functional foods and the like as auxiliary materials, nutritional agents, emulsifying agents and the like of various oral and pharmaceutical preparations.
Description
Technical Field
The invention relates to the technical field of soybean lecithin preparation, in particular to soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio and a preparation method thereof.
Technical Field
The soybean lecithin is a product extracted and processed from the oil residue of soybean oil, has high nutritive value and physiological activity, and is also an excellent natural emulsifier, so that the soybean lecithin is widely used in the industries of food, feed, medicine, chemical industry and the like. Generally, the soybean lecithin comprises the following components in percentage by mass: 17-21% of phosphatidylcholine (namely lecithin, PC), 11-18% of Phosphatidylethanolamine (PE), 16-21% of Phosphatidylinositol (PI), 5-11% of other phospholipids, 35-40% of soybean oil, 2-5% of sterols and other compounds and 4-9% of saccharide compounds, wherein the ratio of Phosphatidylcholine (PC) to Phosphatidylethanolamine (PE) is 1.3-1.6, the ratio of PC and PE is smaller, the HLB value is small, and the hydrophilic emulsification performance is low; in addition, soybean phospholipids also contain structural sugar and free sugar components of heat source substances, the structural sugar is mainly sugar esters, such as monogalactose fatty acid monoglyceride, monogalactose fatty acid diglyceride and the like, the free sugar comprises stachyose, raffinose, sucrose and other oligosaccharides, the existence of the sugar components can have adverse effects on the quality of the phospholipids, for example, maillard reaction of the sugar substances can occur due to heating in the phospholipid processing process to cause browning, so that the application of the phospholipids in the field of food industry is greatly limited, and in addition, if sugar exists during intravenous transfusion, transfusion reaction is likely to occur, and the life safety of patients is endangered.
At present, the development of phosphatidylcholine in soybean phospholipid component is focused on improving the hydrophilic emulsifying property, and the removal of phospholipid saccharide component is mostly ignored. The method for extracting phosphatidylcholine at the present stage mainly comprises the following steps: supercritical fluid extraction, column chromatography and solvent extraction are expensive and have severe operating conditions, and are not suitable for large-scale popularization. The column chromatography is difficult to enlarge, has large equipment investment and is not suitable for large-scale industrialized production. Solvent extraction is the most commonly used method for preparing phosphatidylcholine in industry, but the purity of the product prepared by the traditional solvent extraction method is lower.
The Chinese patent publication No. CN101671359B discloses a method for preparing high-purity soybean lecithin by solvent extraction, which takes soybean concentrated phospholipid as a raw material, obtains soybean powder phospholipid by acetone deoiling, and prepares soybean lecithin with the phosphatidylcholine content of more than or equal to 70% by weight through the procedures of alcohol extraction, acetone-alcohol mixed solvent extraction and the like.
The Chinese patent publication No. CN1390843A discloses a method for extracting phosphatidylcholine from powder soybean lecithin, which adopts a mixed solvent extraction process of acetonitrile and low-carbon alcohol to prepare phosphatidylcholine with the content of 70 percent, and the application of the phosphatidylcholine product is difficult to remove due to the strong toxicity of acetonitrile.
Disclosure of Invention
The invention provides a soybean lecithin with high PC/PE ratio and a preparation method thereof, wherein the soybean lecithin is deoiled by adopting an alcohol-water mixed solvent, the solvent is safe and nontoxic, the deoiling effect is good, the deoiled lecithin is prepared by processes of ethanol extraction, low-temperature freeze separation, a heat removal source, vacuum centrifugal film concentration, low-temperature vacuum drying and the like, the soybean lecithin has high purity, the PC/PE ratio is high, the soybean lecithin does not contain heat source components and harmful solvents, and the soybean lecithin can be widely applied to industries of medicines, health-care foods, functional foods and the like as auxiliary materials, nutritional agents, emulsifying agents and the like of various oral and pharmaceutical preparations.
In order to solve the technical problems, the invention adopts a technical scheme that: the preparation method of the soybean lecithin with high PC/PE ratio comprises the following steps:
(1) Deoiling: taking concentrated soybean phospholipid as a raw material, adopting an alcohol-water mixed solvent to stir, extract and deoil, centrifugally separating to obtain a lower insoluble substance to obtain deoiled phospholipid, wherein the upper liquid part is an oil extraction liquid, and recovering the solvent and the oil through evaporation;
(2) High-efficiency mixed extraction: adding ethanol into the deoiled phospholipid obtained in the step (1), introducing a static mixer for efficient mixed extraction, introducing the material subjected to mixed extraction by the static mixer into a stirring extraction tank for stirring extraction, returning the stirred and extracted material to the static mixer through a pipeline, repeating the above processes for cyclic extraction, centrifuging to separate an extract and insoluble matters after the cyclic extraction is completed, repeatedly extracting the insoluble matters at the lower layer at least once, merging the extract, and drying the separated insoluble matters to recover the solvent and the alcohol insoluble phospholipid;
(3) Cryogenic separation: performing low-temperature crystallization precipitation on the extract obtained in the step (2), filtering to obtain supernatant, and feeding the filtered supernatant into a temporary storage tank;
(4) And (3) heat removal source: pumping the supernatant in the temporary storage tank in the step (3) into an active carbon adsorption tower with temperature control to remove heat source components through adsorption, obtaining filtrate through membrane filtration, and feeding the filtrate after membrane filtration into a next temporary storage tank;
(5) Vacuum centrifugation thin film concentration: concentrating the filtrate obtained in the step (4) in a vacuum state by using a centrifugal film, and concentrating to obtain desolventized soybean lecithin with the ethanol content less than or equal to 5%;
(6) And (5) low-temperature vacuum drying: and (3) further drying and desolventizing the desolventized soybean lecithin obtained in the step (5) in a vacuum state to obtain the transparent soybean lecithin with high PC/PE ratio, wherein the ethanol residual quantity is less than or equal to 10 mg/kg.
Preferably, the alcohol-water mixed solvent in the step (1) comprises ethanol and distilled water, and the volume ratio of the ethanol to the distilled water is 1: 0.1-1.5, adopting a mixed solvent consisting of nontoxic and environment-friendly ethanol and distilled water as a deoiling solvent, and has low cost, high safety, good deoiling effect can be obtained by reasonably controlling the proportion of the ethanol and the distilled water, and the loss of phospholipid is less; the ratio of the mass of the concentrated soybean phospholipid to the volume of the alcohol-water mixed solvent in the step (1) is 1: 0.5-12, wherein the unit is kg/L, the extraction temperature is 20-70 ℃, the stirring speed is 30-400 r/min, the stirring time is 10-90min, the extraction of grease can be accelerated by reasonably controlling the extraction conditions, meanwhile, emulsification is avoided, and a better separation effect is ensured.
Preferably, the ratio of the mass of the deoiled phospholipid to the volume of ethanol in step (2) is 1: 0.5-12, wherein the unit is kg/L, more preferably, the volume percentage concentration of the ethanol is more than 90%, and the mass of the deoiled phospholipid is the theoretical mass after deoiling.
Preferably, the crystallization and precipitation temperature in the step (3) is-10 ℃ to-30 ℃, the stirring speed is 5-80 r/min, and the crystallization and precipitation time is 8-48 h.
Preferably, the temperature of the heat removal source in the step (4) is controlled to be 15-60 ℃.
Preferably, in the step (5), the concentration temperature of the vacuum centrifugal film is 40-90 ℃, the rotation speed of the centrifugal film is 1000-3000 r/min, and the vacuum degree is more than or equal to 0.095MPa.
Preferably, in the step (6), the drying temperature is 45-95 ℃, and the vacuum degree is more than or equal to 0.095MPa.
Preferably, the centrifugal separation device in the step (1) is a disk centrifuge, a tube centrifuge or a horizontal screw centrifuge, and the centrifugal separation device in the step (2) is a disk centrifuge, a tube centrifuge or a horizontal screw centrifuge.
Preferably, the low-temperature freezing separation device in the step (3) is a cooling crystallization tank, the medium-vacuum centrifugal concentration device in the step (5) is a centrifugal thin film vacuum evaporator, and the low-temperature vacuum drying device in the step (6) is a low-temperature thin film dryer.
In order to solve the technical problems, the invention adopts another technical scheme that: the soybean lecithin with high PC/PE ratio is prepared by the preparation method of the soybean lecithin with high PC/PE ratio, and the ratio of PC to PE in the soybean lecithin is 3.5-8.0.
The beneficial effects of the invention are as follows: (1) The invention creatively adopts the mixed solvent consisting of non-toxic and environment-friendly ethanol and distilled water as the deoiling solvent, extracts and deoils the concentrated soybean lecithin, achieves better deoiling effect by reasonably controlling the extraction conditions, and has the advantages of no acetone residue harmful to human bodies, low cost and no toxicity;
(2) Compared with the traditional stirring and mixing extraction, the invention creatively adopts the efficient mixing and circulating extraction process, has high extraction efficiency and high yield of phospholipid in the extract liquid;
(3) According to the invention, a cooling crystallization tank is creatively adopted to crystallize and precipitate insoluble matters in the extract liquid under the conditions of-10 ℃ to-30 ℃ and a stirring speed of 5-80 r/min, and compared with the existing technology of standing low-temperature freezing to crystallize and precipitate insoluble matters in the extract liquid, the insoluble matters can be well crystallized and separated out, and the high-purity phosphatidylcholine is obtained, namely the product has high purity and the ratio of PC to PE is large;
(4) The active carbon adsorption tower is adopted to remove heat source components in the product, the prepared lecithin does not contain the heat source components, and can not cause infusion reaction of patients when being used as a fat emulsion emulsifier, and the high PC/PE product prepared by the active carbon adsorption tower for removing heat source is superior to the alumina column chromatography, alumina adsorption purification and heat source removal technology in the prior art, so that the product quality is remarkably improved;
(5) The invention adopts the centrifugal film vacuum evaporator to concentrate and desolventize, the peripheral distribution effect of the centrifugal force on the solution causes the material to form a liquid film on the heating surface, the evaporation effect is good, the material can be concentrated and desolventized rapidly, and the material is dried in a vacuum state by a low-temperature thin-layer dryer after being concentrated and desolventized, and the solvent residue is less.
(6) The method has the advantages of advanced process equipment, easy industrialization and continuous production, easy operation, high productivity, low cost, no use of harmful solvents, no heat source component, high total yield and purity, stable and controllable quality, capability of preparing the soybean lecithin with different PC/PE values, capability of meeting the requirements of various industries and environmental protection.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
Weighing 50kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 59.4% in a stirring extraction tank, adding 300L of alcohol-water mixed solvent, which is mixed solvent formed by ethanol and distilled water in a proportion of 85:15 (v/v), carrying out mixed extraction for 90min at a temperature of 60 ℃ and a stirring speed of 400r/min, separating by a disk centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 89.2%, introducing the obtained deoiled phospholipid and 150L of ethanol with volume percentage concentration of 95% into the stirring extraction tank provided with a static mixer device, carrying out cyclic extraction for 45min, separating by a disk centrifuge to obtain extract and lower insoluble matter, repeatedly extracting the lower insoluble matter once, combining the extract twice, adding the extract into a cooling crystallization tank with a stirring speed of 40r/min and a cooling crystallization precipitation time of-20 ℃, carrying out filtration to remove the insoluble matter to obtain supernatant, pumping the supernatant into an active carbon adsorption tower component with a temperature of 35 ℃, carrying out filtration membrane removal to obtain filtrate, carrying out vacuum film dehydration at a vacuum concentration of PE (PE) of 0.095MPa for a vacuum film with a temperature of 95 ℃ and a vacuum concentration of soybean lecithin of 95MPa for a vacuum drying at a vacuum of 0.095MPa, and a vacuum concentration of soybean lecithin of low temperature of 95MPa.
The high pressure liquid chromatography analysis results show that: the weight percentage of Phosphatidylcholine (PC) was 71.3%, the weight percentage of Phosphatidylethanolamine (PE) was 13.7%, the weight percentage of Phosphatidylinositol (PI) was 10.2%, and the weight percentage of other phospholipids was 4.8%.
Example 2
Weighing 30kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 60.5% in a stirring extraction tank, adding 280L of alcohol-water mixed solvent, which is mixed solvent formed by ethanol and distilled water in a proportion of 70:30 (v/v), carrying out mixed extraction for 30min at 45 ℃ and a stirring speed of 300r/min, separating by a horizontal spiral centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 91.2%, introducing the obtained deoiled phospholipid and 120L of ethanol with volume percentage concentration of 95% into a stirring extraction tank provided with a static mixer device, carrying out cyclic extraction for 25min, separating by a disc centrifuge to obtain extract and lower insoluble matter, repeatedly extracting the lower insoluble matter once again, combining the extract twice, adding the extract into a cooling crystallization tank with a stirring speed of 35r/min and a cooling crystallization precipitation time of-28 ℃, carrying out filtration to remove the insoluble matter to obtain supernatant, pumping the supernatant into an active carbon adsorption tower with a temperature of 40 ℃ to remove the deoiled phospholipid, filtering membrane with a filter membrane filtration to obtain filtrate with a vacuum concentration of PE (PE) of 0.096 MPa, and a vacuum drying temperature of the vacuum soybean lecithin of 40 MPa at a vacuum concentration of low temperature of 80.096 MPa at a vacuum of 1500 ℃ for drying of the soybean lecithin of vacuum of low temperature of 80 MPa.
The high pressure liquid chromatography analysis results show that: the weight percentage of Phosphatidylcholine (PC) was 78.6%, the weight percentage of Phosphatidylethanolamine (PE) was 12.1%, and the weight percentage of Phosphatidylinositol (PI) and other phospholipids was 9.3%.
Example 3
Weighing 100kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 60.5% in a stirring extraction tank, adding 800L of alcohol-water mixed solvent, which is mixed solvent formed by ethanol and distilled water in a ratio of 60:40 (v/v), carrying out mixed extraction for 60min at 35 ℃ and a stirring speed of 150r/min, separating by a butterfly centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 92.7%, introducing the obtained deoiled phospholipid and 450L of ethanol with volume percentage concentration of 93% into a stirring extraction tank provided with a static mixer device, carrying out cyclic extraction for 25min, separating by a disc centrifuge to obtain extract and lower insoluble matter, carrying out repeated extraction on the lower insoluble matter, merging the extract twice, adding the extract into a cooling crystallization tank with the stirring speed of 35r/min and the temperature of minus 28 ℃, carrying out crystallization precipitation for 24h, carrying out filtration to remove the insoluble matter, pumping the supernatant into an active carbon adsorption tower with the temperature of 35 ℃ to remove the deoiled phospholipid, carrying out filtration membrane filtration to obtain filtrate, carrying out vacuum drying at the temperature of 0.097 MPa for a vacuum concentration of soybean lecithin of low temperature of 1200 MPa and vacuum drying at the temperature of 0.098 MPa for a vacuum concentration of the soybean lecithin of low temperature of 1200.098 MPa, and vacuum drying temperature of the obtained by a vacuum membrane is carried out vacuum drying of soybean lecithin.
The high pressure liquid chromatography analysis results show that: the weight percentage of Phosphatidylcholine (PC) was 85.0%, the weight percentage of Phosphatidylethanolamine (PE) was 10.9%, and the weight percentage of Phosphatidylinositol (PI) and other phospholipids was 4.1%.
Example 4
Weighing 100kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 62.8%, placing in a stirring extraction tank, adding 500L of alcohol-water mixed solvent which is formed by ethanol and distilled water according to the proportion of 55:45 (v/v), mixing and extracting for 80min at 40 ℃ under the condition of stirring speed of 80r/min, separating by a horizontal spiral centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 93.6%, introducing the obtained deoiled phospholipid and 650L of ethanol with volume percentage concentration of 95% into a stirring extraction tank provided with a static mixer device, circularly extracting for 45min, separating by the horizontal spiral centrifuge to obtain extract and lower insoluble matter, repeatedly extracting the lower insoluble matter once, mixing the two extractive solutions, adding the extractive solution into a cooling crystallization tank with stirring speed of 30r/min and temperature of-28deg.C, crystallizing and precipitating for 30 hr, filtering to remove insoluble substances to obtain supernatant, pumping the supernatant into an active carbon adsorption tower with temperature of 60deg.C to remove heat source components, filtering the filtrate with a filter membrane to obtain filtrate, concentrating and desolventizing under vacuum degree of 0.095MPa and temperature of 85deg.C and centrifugal membrane rotation speed of 1500r/min, and drying the desolventized soybean lecithin in a low temperature thin layer dryer with vacuum degree of 0.095MPa and temperature of 95deg.C for 35min to obtain transparent soybean lecithin with PC/PE of 7.6.
The high pressure liquid chromatography analysis results show that: the weight percentage of Phosphatidylcholine (PC) was 85.1%, the weight percentage of Phosphatidylethanolamine (PE) was 11.2%, and the weight percentage of Phosphatidylinositol (PI) and other phospholipids was 3.7%.
Example 5
Weighing 100kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 59.5% in a stirring extraction tank, adding 100L of alcohol-water mixed solvent, which is mixed solvent formed by ethanol and distilled water in a proportion of 45:55 (v/v), carrying out mixed extraction for 50min at 35 ℃ and a stirring speed of 300r/min, separating by a butterfly centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 90.2%, introducing the obtained deoiled phospholipid and 500L of ethanol with volume percentage concentration of 93% into a stirring extraction tank provided with a static mixer device, carrying out cyclic extraction for 30min, separating by a butterfly centrifuge to obtain extract and lower insoluble matter, carrying out repeated extraction on the lower insoluble matter, merging the extract twice, carrying out crystallization precipitation in a cooling crystallization tank with the stirring speed of 80r/min and the temperature of-25 ℃, carrying out filtration to remove the insoluble matter to obtain supernatant, pumping the supernatant into an active carbon adsorption tower with the temperature of 30 ℃ to remove the deoiled phospholipid, carrying out filtration membrane filtration to obtain filtrate, carrying out vacuum drying at the vacuum concentration of PE (PE) of 0.097 MPa at the temperature of 0.80 MPa for 0.093 min, and vacuum drying soybean lecithin at the temperature of 0.097 MPa, and vacuum concentration of the vacuum temperature of the vacuum film of the vacuum soybean lecithin is obtained after the vacuum concentration of the vacuum soybean lecithin is obtained.
The high pressure liquid chromatography analysis results show that: the weight percentage of Phosphatidylcholine (PC) was 52.5%, the weight percentage of Phosphatidylethanolamine (PE) was 14.2%, the weight percentage of Phosphatidylinositol (PI) was 21.7%, and the weight percentage of other phospholipids was 11.6%.
Example 6
Weighing 100kg of concentrated soybean phospholipid raw material with acetone insoluble matter of 60.5%, placing in a stirring extraction tank, adding 1200L of alcohol-water mixed solvent which is mixed solvent of ethanol and distilled water according to the proportion of 90:10 (v/v), mixing and extracting for 15min at 20 ℃ under the condition of stirring speed of 30r/min, separating by a butterfly centrifuge to obtain deoiled phospholipid with acetone insoluble matter of 71.3%, introducing the obtained deoiled phospholipid and 800L of ethanol with volume percentage concentration of 95% into a stirring extraction tank provided with a static mixer device, circularly extracting for 45min, separating by a butterfly centrifuge to obtain extract and lower insoluble matter, repeatedly extracting the lower insoluble matter once, mixing the two extractive solutions, adding the extractive solution into a cooling crystallization tank with stirring speed of 15r/min and temperature of-10deg.C, crystallizing and precipitating for 12 hr, filtering to remove insoluble substances to obtain supernatant, pumping the supernatant into an active carbon adsorption tower with temperature of 20deg.C to remove heat source components, filtering the filtrate with a filter membrane to obtain filtrate, concentrating and desolventizing under vacuum degree of 0.095MPa and temperature of 50deg.C and centrifugal membrane rotation speed of 3000r/min, and drying the desolventized soybean lecithin in a low-temperature thin-layer dryer with vacuum degree of 0.095MPa and temperature of 45deg.C for 150min to obtain transparent soybean lecithin with PC/PE of 3.5.
The high pressure liquid chromatography analysis results show that: 45.8% by weight of Phosphatidylcholine (PC), 13.1% by weight of Phosphatidylethanolamine (PE), 23.8% by weight of Phosphatidylinositol (PI) and 17.3% by weight of other phospholipids.
Comparative example 1
Taking 50kg of concentrated soybean phospholipid raw material with 59.6% of acetone insoluble matters and 300L of ethanol with 95% of volume percentage concentration, introducing the concentrated soybean phospholipid raw material into a stirring extraction tank provided with a static mixer device, circularly extracting for 45min, separating the mixture by a butterfly centrifuge to obtain an extract and a lower insoluble matters, repeatedly extracting the lower insoluble matters once again, combining the two extracts, adding the extract into a cooling crystallization tank with the stirring speed of 40r/min and the temperature of-20 ℃ for crystallization and precipitation for 30h, filtering to remove insoluble matters to obtain supernatant, pumping the supernatant into an active carbon adsorption tower with the temperature of 35 ℃ to remove heat source components, filtering the obtained filtrate by a filter membrane, concentrating and desolventizing the filtrate by a centrifugal film vacuum evaporator under the conditions of the vacuum degree of 0.095MPa and the centrifugal film rotating speed of 1500r/min, and drying the desolventized soybean lecithin by a low-temperature dryer with the vacuum degree of 0.095MPa and the temperature of 90 ℃ for 40min to obtain transparent soybean lecithin with the PC/PE 2.2 containing 45.8% of acetone insoluble matters.
The high pressure liquid chromatography analysis results show that: 41.6% by weight of Phosphatidylcholine (PC), 18.9% by weight of Phosphatidylethanolamine (PE), 21.6% by weight of Phosphatidylinositol (PI) and 17.9% by weight of other phospholipids.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The preparation method of the soybean lecithin is characterized by comprising the following steps:
(1) Deoiling: extracting and deoiling concentrated soybean phospholipid as a raw material by adopting an alcohol-water mixed solvent, and centrifugally separating to obtain a lower insoluble substance to obtain the deoiled phospholipid, wherein the alcohol-water mixed solvent consists of ethanol and distilled water, and the volume ratio of the ethanol to the distilled water is 17:3, 7:3, 3:2, 11:9 and 9:11 or 9:1;
(2) Mixing and extracting: adding ethanol into the deoiled phospholipid obtained in the step (1), introducing the mixture into a static mixer for mixed extraction, allowing the material subjected to mixed extraction by the static mixer to enter a stirring extraction tank for stirring extraction, returning the stirred and extracted material to the static mixer through a pipeline, repeating the above processes for cyclic extraction, centrifuging to separate extract liquid and insoluble matters after the cyclic extraction is completed, repeatedly extracting the insoluble matters at the lower layer at least once, and combining the extract liquid;
(3) Freezing and separating: performing low-temperature crystallization and precipitation on the extract liquid obtained in the step (2), wherein the low-temperature crystallization and precipitation temperature is-10 ℃ to-30 ℃, and filtering to obtain supernatant;
(4) Depyrogenation: pumping the supernatant obtained in the step (3) into an active carbon adsorption tower to remove pyrogen components, and filtering by a membrane to obtain filtrate;
(5) Vacuum centrifugation thin film concentration: performing centrifugal thin film evaporation concentration on the filtrate obtained in the step (4) in a vacuum state, and concentrating to obtain desolventized soybean lecithin;
(6) And (5) low-temperature vacuum drying: drying and desolventizing the desolventized soybean lecithin obtained in the step (5) in a vacuum state to obtain the soybean lecithin, wherein the low-temperature vacuum drying temperature is 45-95 ℃, and the vacuum degree is more than or equal to 0.095MPa.
2. The method for preparing soybean lecithin according to claim 1, wherein: the ratio of the mass of the concentrated soybean phospholipid to the volume of the alcohol-water mixed solvent in the step (1) is 1: 0.5-12, wherein the unit of the ratio of the mass of the concentrated soybean phospholipid to the volume of the pure water mixed solvent is kg/L, the extraction temperature is 20-70 ℃, the stirring speed is 30-400 r/min, and the stirring time is 10-90min.
3. The method for preparing soybean lecithin according to claim 1, wherein: the ratio of the mass of the deoiled phospholipid to the volume of the ethanol in the step (2) is 1: and 0.5-12, wherein the unit of the ratio of the mass of the deoiled phospholipid to the volume of the ethanol is kg/L.
4. The method for preparing soybean lecithin according to claim 1, wherein: the stirring speed in the step (3) is 5-80 r/min, and the crystallization and precipitation time is 8-48 h.
5. The method for preparing soybean lecithin according to claim 1, wherein: the depyrogenation temperature in the step (4) is 15-60 ℃.
6. The method for preparing soybean lecithin according to claim 1, wherein: the concentration temperature of the vacuum centrifugal film in the step (5) is 40-90 ℃, the rotation speed of the centrifugal film is 1000-3000 r/min, and the vacuum degree is more than or equal to 0.095MPa.
7. The method for preparing soybean lecithin according to claim 1, wherein: the centrifugal separation equipment in the step (1) is a disc centrifuge, a tube centrifuge or a horizontal screw centrifuge, and the centrifugal separation equipment in the step (2) is a disc centrifuge, a tube centrifuge or a horizontal screw centrifuge.
8. The method for preparing soybean lecithin according to claim 1, wherein: the freezing separation equipment in the step (3) is a cooling crystallization tank, the vacuum centrifugal film concentration equipment in the step (5) is a centrifugal film vacuum evaporator, and the low-temperature vacuum drying equipment in the step (6) is a low-temperature thin-layer dryer.
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