CN109438508A - A kind of preparation method of phosphatidyl-ethanolamine - Google Patents
A kind of preparation method of phosphatidyl-ethanolamine Download PDFInfo
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- JZNWSCPGTDBMEW-UHFFFAOYSA-N Glycerophosphorylethanolamin Natural products NCCOP(O)(=O)OCC(O)CO JZNWSCPGTDBMEW-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 150000008104 phosphatidylethanolamines Chemical class 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 146
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000012141 concentrate Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 13
- 238000013517 stratification Methods 0.000 claims abstract description 13
- 239000000787 lecithin Substances 0.000 claims abstract description 12
- 235000010445 lecithin Nutrition 0.000 claims abstract description 12
- 238000003808 methanol extraction Methods 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 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 claims abstract description 8
- 229940067606 lecithin Drugs 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 244000068988 Glycine max Species 0.000 claims description 6
- 235000010469 Glycine max Nutrition 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910001424 calcium ion Inorganic materials 0.000 claims description 2
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 235000020238 sunflower seed Nutrition 0.000 claims description 2
- 102000002322 Egg Proteins Human genes 0.000 claims 1
- 108010000912 Egg Proteins Proteins 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 210000004681 ovum Anatomy 0.000 claims 1
- 150000003904 phospholipids Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 11
- -1 phospholipids compounds Chemical class 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XOKJUJMYGNKBTR-UHFFFAOYSA-L CO.Cl[Mg]Cl Chemical compound CO.Cl[Mg]Cl XOKJUJMYGNKBTR-UHFFFAOYSA-L 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 description 2
- BOKSKTADHYXBBM-UHFFFAOYSA-L [Cl-].[Cl-].[Zn+2].OC Chemical compound [Cl-].[Cl-].[Zn+2].OC BOKSKTADHYXBBM-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 229940031098 ethanolamine Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N monoethanolamine hydrochloride Natural products NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 239000000825 pharmaceutical preparation Substances 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- PORPENFLTBBHSG-MGBGTMOVSA-N 1,2-dihexadecanoyl-sn-glycerol-3-phosphate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(O)=O)OC(=O)CCCCCCCCCCCCCCC PORPENFLTBBHSG-MGBGTMOVSA-N 0.000 description 1
- CFWRDBDJAOHXSH-SECBINFHSA-N 2-azaniumylethyl [(2r)-2,3-diacetyloxypropyl] phosphate Chemical compound CC(=O)OC[C@@H](OC(C)=O)COP(O)(=O)OCCN CFWRDBDJAOHXSH-SECBINFHSA-N 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
- 241000208818 Helianthus Species 0.000 description 1
- 235000003222 Helianthus annuus Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- QSLUWZMIMXNLJV-UHFFFAOYSA-L calcium methanol dichloride Chemical compound [Cl-].[Cl-].[Ca+2].OC QSLUWZMIMXNLJV-UHFFFAOYSA-L 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
- 230000004065 mitochondrial dysfunction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940042880 natural phospholipid Drugs 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 125000001095 phosphatidyl group Chemical group 0.000 description 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 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
Landscapes
- 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)
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of phosphatidyl-ethanolamine, comprising the following steps: (1) chooses crude lecithin, evaporated under reduced pressure solvent after fatty alcohol aqueous solution stirring extraction is added, obtains concentrate；(2) step (1) resulting concentrate is dissolved in methanol and obtains phosphatide methanol solution, the stirring extraction of divalent metal salt methanol solution is then added, obtains methanol extraction liquid；(3) methanol extraction liquid is mixed, heating stirring with non-polar macroporous resin, obtains the upper layer methanol stillness of night after stratification, will filtered after methanol stillness of night cooling crystallization, by filter vacuum drying to obtain phosphatidyl-ethanolamine；The preparation method concise in technology, cost and energy consumption are lower, safety, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to phosphatide techniques, and in particular to a kind of preparation method of phosphatidyl-ethanolamine.
Background technique
Phosphatidyl-ethanolamine (PE) is a kind of important phospholipids compounds, also known as cephalin, present in living nature
In phosphatide, content is only second to phosphatidyl second choline (PC), is concerned, getting up early application due to its special physiological action
In field of food industry, with the continuous deepening of research, function and application range also constantly expand therewith, especially high-purity
Phosphatidyl-ethanolamine be even more gradually applied to field of pharmaceutical preparations, can be used as the emulsifier and liposome preparation of pharmaceutical preparation
Auxiliary material, it may also be used for adjust mitochondrial dysfunction, treat the functions such as depression and anxiety disorder.Existing report about phosphatide
Acyl ethanol amine has animals and plants to extract in conjunction with column chromatography, chemical synthesis and enzyme catalysis method.Animals and plants extraction method such as patent
The natural phospholipid acyl that method disclosed in CN201410841454.1, CN10038618C and CN201510395419.6 obtains
Ethyl alcohol amine content is lower, and consumption of organic solvent is big, and technique is cumbersome, and it is big to purify required amount of filler, with high costs, and manually closes
At phosphatidyl-ethanolamine such as patent CN201210430649.8 and CN201010137564.1, technique in actual production because
Low yield and be difficult to realize, and because using phosphorus oxychloride in technique, the noxious materials such as phosphorus trichloride and sodium azide and should not examine
Consider, furthermore enzyme process catalysis method has mild condition, and simple process is easy to operate and the more low advantage of Costco Wholesale, but studies still not
It is deep enough.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of phosphatidyl-ethanolamine, the preparation method concise in technology, at
This and energy consumption are lower, safety, it is easy to accomplish industrialized production, and the phosphatidyl-ethanolamine purity is high obtained.
Above-mentioned purpose of the invention is achieved through the following technical solutions: a kind of preparation side of phosphatidyl-ethanolamine
Method, comprising the following steps:
(1) crude lecithin is chosen, evaporated under reduced pressure solvent after fatty alcohol aqueous solution stirring extraction is added, obtains concentrate；
(2) step (1) resulting concentrate is dissolved in methanol and obtains phosphatide methanol solution, it is molten that divalent metal salt methanol is then added
Liquid stirring extraction, obtains methanol extraction liquid；
(3) methanol extraction liquid is mixed, heating stirring with non-polar macroporous resin, obtains the upper layer methanol stillness of night after stratification,
It will be filtered after methanol stillness of night cooling crystallization, by filter vacuum drying to obtain phosphatidyl-ethanolamine.
In the preparation method of above-mentioned phosphatidyl-ethanolamine:
Preferably, crude lecithin as described in step (1) derives from soybean or sunflower seeds.
Phosphatidic acid, sugar, phosphatidyl-ethanolamine, phosphatidyl choline are usually contained in crude lecithin, there are also some other phosphorus
Ester compounds, wherein the content of phosphatidyl-ethanolamine is about 10% or so.
Preferably, fatty alcohol as described in step (1) is ethyl alcohol or isopropanol；Fatty alcohol in the fatty alcohol aqueous solution
Volumn concentration be 85 ~ 95%, the volume ratio of the fatty alcohol aqueous solution and crude lecithin is 4 ~ 6mL:1g.
The effect enrichment acid acyl ethanol amine of fatty alcohol aqueous solution.
Preferably, the pH value of fatty alcohol aqueous solution described in step (1) is 7 ~ 9, and temperature is 50 ~ 70 DEG C when stirring extracts,
Stirring extraction time is 4 ~ 8h.
Preferably, the dosage relation of methanol described in step (2) and concentrate is 3 ~ 5mL:1g.
Preferably, bivalent metal ion is zinc ion, magnesium ion and calcium ion in divalent metal salt described in step (2)
One of.
The effect of divalent metal salt methanol solution is to remove phosphate acid ester.
Preferably, the mass percentage of the diformazan metal salt in the methanol solution of divalent metal salt described in step (2)
It is 40 ~ 55%, the volume ratio of the methanol solution of the divalent metal salt and the phosphatide methanol solution is 1:1 ~ 2:1, stirring extraction
Shi Wendu is 20 ~ 30 DEG C, and the time is 5 ~ 10h.
Preferably, non-polar macroporous resin described in step (3) is selected from HP-20 non-polar macroporous resin or the non-pole D101
Property macroreticular resin.
Preferably, the volume ratio of methanol extraction liquid described in step (3) and the non-polar macroporous resin be 1:1 ~
2:1, temperature is 30 ~ 40 DEG C when heating stirring, and the heating stirring time is 5 ~ 10 hours.
The effect of non-polar macroporous resin is to remove small polar impurity.
Preferably, the crystallization temperature of the methanol stillness of night described in step (3) is -10 ~ 0 DEG C, and the crystallization time is 12 ~ 18 hours.
The effect of crystallization is to remove the big polar phosphoric ester compound in part.
The invention has the following advantages:
(1) raw material used in the present invention is crude lecithin, thus cheap；
(2) the preparation method integrated artistic of phosphatidyl-ethanolamine of the present invention is succinct, and mild condition, overall cost is lower, is easy to real
It now industrializes, 55% or more phosphatidylethanolamine content obtained, purity is higher；
(3) raw material first passes through preparatory purifying in the preparation method of phosphatidyl-ethanolamine of the present invention, then carries out resin adsorption and purifying,
Concise in technology, energy consumption is lower, advantages of nontoxic raw materials, and resin is renewable and reuses, it is easy to accomplish industrialized production, to China's phosphatide
Industry, health food and pharmaceutical industries will all be of great significance.
Specific embodiment
The present invention, but the scope of protection of present invention not office are further illustrated below in conjunction with specific embodiment
Limit and following embodiments.
Embodiment 1
The preparation method of phosphatidyl-ethanolamine provided in this embodiment, comprising the following steps:
100 grams of sunflower phosphatides are extracted 8 hours in 85% ethanol solution, 70 DEG C of stirrings that 400 milliliters of pH are 8, evaporated under reduced pressure second
Alcohol extract liquor obtains 46 grams of concentrates；
46 grams of concentrates are dissolved in 225 ml methanols, be then added isometric concentration be 55% zinc chloride methanol solution and in
Temperature is 20 DEG C of stirring 5h, obtains about 500 milliliters of methanol extraction liquid after stratification；
250 milliliters of macroreticular resin HP-20 is then added and is stirred 5 hours in 30 DEG C, it is clear that upper layer methanol is obtained after stratification
The methanol stillness of night is cooled to 0 DEG C of crystallization, is obtained by filtration methanol solution (i.e. filtrate) after being kept for 12 hours, is concentrated in vacuo methanol solution by night
Totally 14 grams of phosphatidyl-ethanolamine are obtained after drying, content is 57% after HPLC measurement and standard control.
Embodiment 2
The preparation method of phosphatidyl-ethanolamine provided in this embodiment, comprising the following steps:
100 grams of Crude soybean lecithins are extracted 4 hours in 95% aqueous isopropanol, 50 DEG C of stirrings that 600 milliliters of pH are 9, decompression is steamed
Dry isopropyl alcohol extraction liquid obtains 50 grams of concentrates；
50 grams of concentrates are dissolved in 250 ml methanols, the magnesium chloride methanol solution that then 2 times of volumetric concentrations of addition are 40% is simultaneously
It is 30 DEG C of stirring 10h in temperature, obtains about 750 milliliters of methanol extraction liquid after stratification；
375 milliliters of macroreticular resin D101 is then added and is stirred 10 hours in 40 DEG C, it is clear that upper layer methanol is obtained after stratification
Night.The methanol stillness of night is cooled to -10 DEG C of crystallizations, methanol solution is obtained by filtration after being kept for 18 hours, after vacuum concentration methanol solution is dry
Totally 11 grams of phosphatidyl-ethanolamine are obtained, content is 55% after HPLC measurement and standard control.
Embodiment 3
The preparation method of phosphatidyl-ethanolamine provided in this embodiment, comprising the following steps:
100 grams of Crude soybean lecithins are extracted 6 hours in 90% ethanol solution, 60 DEG C of stirrings that 500 milliliters of pH are 8, evaporated under reduced pressure
Alcohol extraction liquid obtains 47 grams of concentrates；
47 grams of concentrates are dissolved in 141 ml methanols, the calcium chloride methanol solution that then 2 times of volumetric concentrations of addition are 40% is simultaneously
It is 30 DEG C of stirring 8h in temperature, obtains about 470 milliliters of methanol extraction liquid after stratification；
470 milliliters of macroreticular resin HP-20 is then added and is stirred 8 hours in 40 DEG C, it is clear that upper layer methanol is obtained after stratification
Night.The methanol stillness of night is cooled to -5 DEG C of crystallizations, keeps that methanol solution is obtained by filtration within 16 hours, after vacuum concentration methanol solution is dry to obtain the final product
To totally 10 grams of phosphatidyl-ethanolamine, content is 65% after HPLC measurement and standard control.
Embodiment 4
The preparation method of phosphatidyl-ethanolamine provided in this embodiment, comprising the following steps:
100 grams of Crude soybean lecithins are extracted 7 hours in 90% ethanol solution, 65 DEG C of stirrings that 500 milliliters of pH are 8, evaporated under reduced pressure
Alcohol extraction liquid obtains 48 grams of concentrates；
47 grams of concentrates are dissolved in 188 ml methanols, the zinc chloride methanol solution that then 2 times of volumetric concentrations of addition are 50% is simultaneously
It is 25 DEG C of stirring 8h in temperature, obtains about 680 milliliters of methanol extraction liquid after stratification；
680 milliliters of D101 macroreticular resin is then added and is stirred 8 hours in 40 DEG C, it is clear that upper layer methanol is obtained after stratification
Night.The methanol stillness of night is cooled to -5 DEG C of crystallizations, methanol solution is obtained by filtration after being kept for 16 hours, after vacuum concentration methanol solution is dry i.e.
Totally 12 grams of phosphatidyl-ethanolamine are obtained, content is 63% after HPLC measurement and standard control.
Embodiment 5
The preparation method of phosphatidyl-ethanolamine provided in this embodiment, comprising the following steps:
100 grams of Crude soybean lecithins are extracted 7 hours in 95% aqueous isopropanol, 65 DEG C of stirrings that 500 milliliters of pH are 7, decompression is steamed
Dry isopropyl alcohol extraction liquid obtains 52 grams of concentrates；
52 grams of concentrates are dissolved in 208 ml methanols, the magnesium chloride methanol solution that then 2 times of volumetric concentrations of addition are 50% is simultaneously
It is 25 DEG C of stirring 8h in temperature, obtains about 720 milliliters of methanol extraction liquid after stratification；
480 milliliters of macroreticular resin HP-20 is then added and is stirred 8 hours in 40 DEG C, it is clear that upper layer methanol is obtained after stratification
Night.The methanol stillness of night is cooled to -5 DEG C of crystallizations, methanol solution is obtained by filtration after being kept for 16 hours, after vacuum concentration methanol solution is dry i.e.
Totally 13 grams of phosphatidyl-ethanolamine are obtained, content is 62% after HPLC measurement and standard control.
A part of specific embodiment is enumerated above, and the present invention will be described, it is necessary to which indicated herein is specific real up and down
It applies example and is served only for that the present invention is further illustrated, do not represent limiting the scope of the invention.Other people are according to this hair
The bright some nonessential modifications made and adjustment still fall within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of phosphatidyl-ethanolamine, it is characterized in that the following steps are included:
(1) crude lecithin is chosen, evaporated under reduced pressure solvent after fatty alcohol aqueous solution stirring extraction is added, obtains concentrate；
(2) step (1) resulting concentrate is dissolved in methanol and obtains phosphatide methanol solution, it is molten that divalent metal salt methanol is then added
Liquid stirring extraction, obtains methanol extraction liquid；
(3) methanol extraction liquid is mixed, heating stirring with non-polar macroporous resin, obtains the upper layer methanol stillness of night after stratification,
It will be filtered after methanol stillness of night cooling crystallization, by filter vacuum drying to obtain phosphatidyl-ethanolamine.
2. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: thick ovum as described in step (1)
Phospholipid sources are in soybean or sunflower seeds.
3. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: fat as described in step (1)
Alcohol is ethyl alcohol or isopropanol；The volumn concentration of fatty alcohol is 85 ~ 95% in the fatty alcohol aqueous solution, the fatty alcohol
The volume ratio of aqueous solution and crude lecithin is 4 ~ 6mL:1g.
4. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: fatty alcohol described in step (1)
The pH value of aqueous solution is 7 ~ 9, and temperature is 50 ~ 70 DEG C when stirring extracts, and stirring extraction time is 4 ~ 8h.
5. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: methanol described in step (2) with
The dosage relation of concentrate is 3 ~ 5mL:1g.
6. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: divalent described in step (2)
Bivalent metal ion in metal salt is one of zinc ion, magnesium ion and calcium ion.
7. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: divalent described in step (2) is golden
Belong to salt methanol solution in diformazan metal salt mass percentage be 40 ~ 55%, the methanol solution of the divalent metal salt with
The volume ratio of the phosphatide methanol solution is 1:1 ~ 2:1, and temperature is 20 ~ 30 DEG C when stirring extracts, and the time is 5 ~ 10h.
8. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: non-pole described in step (3)
Property macroreticular resin be selected from HP-20 or D101.
9. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: methanol described in step (3)
The volume ratio of extract liquor and the non-polar macroporous resin is 1:1 ~ 2:1, and temperature is 30 ~ 40 DEG C when heating stirring, and heating is stirred
Mixing the time is 5 ~ 10 hours.
10. the preparation method of phosphatidyl-ethanolamine according to claim 1, it is characterized in that: methanol described in step (3) is clear
The crystallization temperature at night is -10 ~ 0 DEG C, and the crystallization time is 12 ~ 18 hours.
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| CN113995763A (en) * | 2021-11-10 | 2022-02-01 | 中南大学湘雅医院 | Application of phosphatidylethanolamine as active ingredient in preparation of psoriasis treatment medicine, psoriasis treatment medicine and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113995763A (en) * | 2021-11-10 | 2022-02-01 | 中南大学湘雅医院 | Application of phosphatidylethanolamine as active ingredient in preparation of psoriasis treatment medicine, psoriasis treatment medicine and preparation method thereof |
| CN113995763B (en) * | 2021-11-10 | 2023-08-11 | 中南大学湘雅医院 | Application of phosphatidylethanolamine as active ingredient in preparation of psoriasis treatment medicine, psoriasis treatment medicine and preparation method thereof |
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