CN107721871A - A kind of method that molecular distillation isolates and purifies konjak ceramide - Google Patents
A kind of method that molecular distillation isolates and purifies konjak ceramide Download PDFInfo
- Publication number
- CN107721871A CN107721871A CN201710999197.8A CN201710999197A CN107721871A CN 107721871 A CN107721871 A CN 107721871A CN 201710999197 A CN201710999197 A CN 201710999197A CN 107721871 A CN107721871 A CN 107721871A
- Authority
- CN
- China
- Prior art keywords
- molecular distillation
- ceramide
- konjak
- grade
- purifies
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- YDNKGFDKKRUKPY-JHOUSYSJSA-N C16 ceramide Natural products CCCCCCCCCCCCCCCC(=O)N[C@@H](CO)[C@H](O)C=CCCCCCCCCCCCCC YDNKGFDKKRUKPY-JHOUSYSJSA-N 0.000 title claims abstract description 45
- 229940106189 ceramide Drugs 0.000 title claims abstract description 45
- ZVEQCJWYRWKARO-UHFFFAOYSA-N ceramide Natural products CCCCCCCCCCCCCCC(O)C(=O)NC(CO)C(O)C=CCCC=C(C)CCCCCCCCC ZVEQCJWYRWKARO-UHFFFAOYSA-N 0.000 title claims abstract description 45
- VVGIYYKRAMHVLU-UHFFFAOYSA-N newbouldiamide Natural products CCCCCCCCCCCCCCCCCCCC(O)C(O)C(O)C(CO)NC(=O)CCCCCCCCCCCCCCCCC VVGIYYKRAMHVLU-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229920002752 Konjac Polymers 0.000 title claims abstract description 44
- 238000000199 molecular distillation Methods 0.000 title claims abstract description 44
- CRJGESKKUOMBCT-VQTJNVASSA-N N-acetylsphinganine Chemical compound CCCCCCCCCCCCCCC[C@@H](O)[C@H](CO)NC(C)=O CRJGESKKUOMBCT-VQTJNVASSA-N 0.000 title claims abstract description 40
- 235000010485 konjac Nutrition 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000004821 distillation Methods 0.000 claims abstract description 10
- 239000012530 fluid Substances 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims description 12
- 230000005494 condensation Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010025 steaming Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- -1 caproyl Chemical group 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 150000003410 sphingosines Chemical class 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000000605 extraction Methods 0.000 description 7
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- NPRJSFWNFTXXQC-QFWQFVLDSA-N N-(hexanoyl)sphing-4-enine Chemical compound CCCCCCCCCCCCC\C=C\[C@@H](O)[C@H](CO)NC(=O)CCCCC NPRJSFWNFTXXQC-QFWQFVLDSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 241001312219 Amorphophallus konjac Species 0.000 description 2
- 235000001206 Amorphophallus rivieri Nutrition 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010898 silica gel chromatography Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 241001278826 Amorphophallus Species 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 208000001953 Hypotension Diseases 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010067868 Skin mass Diseases 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 208000021822 hypotensive Diseases 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 239000000252 konjac Substances 0.000 description 1
- 201000007227 lymph node tuberculosis Diseases 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of method that molecular distillation isolates and purifies konjak ceramide, first by konjak ceramide supercritical CO2After fluid extract preheats in preheater, it is added to through feeder in molecular distillation system, in high vacuum conditions, konjak ceramide carries out quadratic component distillation processing under appropriate purification condition, and final separation obtains the C of higher degree6Ceramide (N caproyl D sphingosines) sample.The present invention is to konjak ceramide supercritical CO2Extract carries out molecular distillation secondary separation purifying, the rational technology, feasible, simple to operate, and no organic reagent residual, purity is high and can have very strong practical value with mass industrialized production.
Description
Technical field
The present invention relates to traditional Chinese medicine extraction separation technology field, more particularly to a kind of molecular distillation to isolate and purify konjaku nerve acyl
The method of amine.
Background technology
Konjaku (Konjac), Araeceae Amorphophallus, for the block of herbaceous plant konjaku (Amorphophalluskonjac)
Stem.Konjaku is cold in nature, pungent, poisonous；Can be promoting blood circulation and removing blood stasis, removing toxicity for detumescence, wide intestines defaecation, resolving phlegm and softening hard masses；Cure mainly hypotensive, it is hypoglycemic,
The disease such as scrofula subcutaneous nodule, the damage stasis of blood swollen, constipation stomachache, abscess of throat, swelling and aching of gum.It is reported that contain in konjaku than more rich
Ceramide, the content of its ceramide are up to 0.15~0.2%, are currently used raw material such as rice bran, soybean, wheats etc.
10 times of raw material.Dihydrophytoceramide is a kind of most in recent years emerging active component, has the effect such as barrier, moisturizing, water holding, with
And the physiologically active such as antitumor, Immune enhancement, there is extensive use value.
At present, it is existing separation, purifying konjak ceramide method have consumption of organic solvent is big, the production cycle is long,
The shortcomings of production cost is high.Chinese patent (application number 201410040856.1) discloses ceramide in a kind of fry starch of konjak
Extraction separation method, this method shakes extraction konjak ceramide first with 95% EtOH Sonicate, through super after extract solution is concentrated
Critical CO2Extraction, extract pass through supercritical CO again2Reextraction, finally give C6- ceramide content is 73.8% production
The problems such as production cycle is long, ethanol consumption is big, equipment cost is high, safety requirements is higher be present in product, still, the technique；It is Chinese special
Sharp (application number 201210133207.7) uses 70% ethanol solution ultrasonic wave extraction konjak ceramide, is used after extract solution concentration
Petroleum ether extraction 3 times, after purified through silica gel column chromatography, with petroleum ether：Ethyl acetate solvent is eluted, after eluent concentration
Purified again through silica gel column chromatography, with ethanol：Water is that solvent is eluted, cold through centrifuge, vacuum after eluent concentration
The sample of dry system is freezed, this method has the problems such as complex production process, consumption of organic solvent are big, production cost is high.
The content of the invention
In order to overcome, prior art ceramide extraction production technology is cumbersome, the production cycle is long, consumption of organic solvent is big, raw
The problems such as cost is high is produced, the present invention provides a kind of method that molecular distillation isolates and purifies konjak ceramide.
The purpose of the present invention is achieved through the following technical solutions：A kind of molecular distillation isolates and purifies the side of konjak ceramide
Method, step are as follows：
Step 1：Weigh appropriate konjak ceramide supercritical CO2Fluid extract, it is added in preheater, heats up
Preheated；
Step 2：By preheated material, I grade of molecular distillation of progress in molecular distillation system is added to through feeder, and
The strictly condition of I grade of molecular distillation of control；
Step 3：By I grade of molecular distillation resulting material, II grade of molecule of progress in molecular distillation system is added to through feeder
Distillation, and the condition of II grade of molecular distillation is strictly controlled, the component flowed out along condensation column is the konjak ceramide of high-purity
Sample.
Preferably, the method that a kind of described molecular distillation isolates and purifies konjak ceramide, in the step 1, konjaku
Ceramide supercritical CO2C in fluid extract6- ceramide content is 10%~20%.
Preferably, the method that a kind of described molecular distillation isolates and purifies konjak ceramide, in the step 1, preheating
Temperature is 60~80 DEG C.
Preferably, the method that a kind of described molecular distillation isolates and purifies konjak ceramide, in the step 2, I grade
Molecular distillation condition is：0.1~10Pa of vacuum, 160~220 DEG C, 1~5ml/min of charging rate of vapo(u)rizing temperature, condensation temperature
0~10 DEG C, 150~400r/min of knifing rotating speed.
Preferably, the method that a kind of described molecular distillation isolates and purifies konjak ceramide, in the step 3, II point
Sub- distillation condition is：20~100Pa of vacuum, 120~160 DEG C, 1~5ml/min of charging rate of vapo(u)rizing temperature, condensation temperature 10
~20 DEG C, 150~350r/min of knifing rotating speed.
Compared with prior art, the present invention has following excellent beneficial effect：The present invention is to konjak ceramide supercritical CO2
Extract carries out molecular distillation secondary separation purifying, the rational technology, feasible, simple to operate, no organic reagent residual, purity height
And there can be very strong practical value with mass industrialized production.
Embodiment
For a better understanding of the present invention, technical scheme will be carried out by embodiment below clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example is applied, belongs to the scope of protection of the invention.
Embodiment 1
A kind of method that molecular distillation isolates and purifies konjak ceramide, step are as follows：
(1) konjak ceramide supercritical CO is weighed2Fluid extract A 50g, are added in preheater, and heating carries out pre-
Heat；
(2) by preheated material, it is 10Pa in vacuum, 220 DEG C, charging rate 1ml/min of vapo(u)rizing temperature, condenses temperature
10 DEG C are spent, I grade of molecular distillation is carried out under conditions of knifing rotating speed 150r/min, obtains I grade of distillation of konjak ceramide, pass through
HPLC methods determine wherein C6- ceramide content is 45.65%.
(3) it is 100Pa in vacuum by I grade of molecular distillation resulting material, 160 DEG C of vapo(u)rizing temperature, charging rate 1ml/
Min, 20 DEG C of condensation temperature, II grade of molecular distillation is carried out under conditions of knifing rotating speed 150r/min, collected along condensation column outflow
Component is II grade of distillation, and wherein C is determined through HPLC methods6- ceramide content content is 75.33%.
Embodiment 2
A kind of method that molecular distillation isolates and purifies konjak ceramide, step are as follows：
(1) konjak ceramide supercritical CO is weighed2Fluid extract B 50g, are added in preheater, and heating carries out pre-
Heat；
(2) by preheated material, it is 5Pa in vacuum, 180 DEG C, charging rate 2ml/min of vapo(u)rizing temperature, condenses temperature
4 DEG C are spent, I grade of molecular distillation is carried out under conditions of knifing rotating speed 250r/min, obtains I grade of distillation of konjak ceramide, pass through
HPLC methods determine wherein C6- ceramide content content is 48.97%.
(3) it is 50Pa in vacuum by I grade of molecular distillation resulting material, 140 DEG C of vapo(u)rizing temperature, charging rate 3ml/
Min, 12 DEG C of condensation temperature, II grade of molecular distillation is carried out under conditions of knifing rotating speed 270r/min, collected along condensation column outflow
Component is II grade of distillation, and wherein C is determined through HPLC methods6- ceramide content content is 77.14%.
Embodiment 3
A kind of method that molecular distillation isolates and purifies konjak ceramide, step are as follows：
(1) konjak ceramide supercritical CO is weighed2Fluid extract C 50g, are added in preheater, and heating carries out pre-
Heat；
(2) by preheated material, it is 0.1Pa in vacuum, 160 DEG C, charging rate 5ml/min of vapo(u)rizing temperature, condenses
0 DEG C of temperature, I grade of molecular distillation is carried out under conditions of knifing rotating speed 400r/min, obtains I grade of distillation of konjak ceramide, passed through
HPLC methods determine wherein C6- ceramide content content is 50.85%.
(3) it is 20Pa in vacuum by I grade of molecular distillation resulting material, 120 DEG C of vapo(u)rizing temperature, charging rate 5ml/
Min, 10 DEG C of condensation temperature, II grade of molecular distillation is carried out under conditions of knifing rotating speed 350r/min, collected along condensation column outflow
Component is II grade of distillation, and wherein C is determined through HPLC methods6- ceramide content content is 78.57%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (5)
1. a kind of method that molecular distillation isolates and purifies konjak ceramide, it is characterised in that step is as follows：
Step 1：Weigh appropriate konjak ceramide supercritical CO2Fluid extract, it is added in preheater, heating carries out pre-
Heat；
Step 2：By preheated material, I grade of molecular distillation of progress in molecular distillation system is added to through feeder, and strictly
Control the condition of I grade of molecular distillation；
Step 3：By I grade of molecular distillation resulting material, it is added to through feeder in molecular distillation system and carries out II grade of molecule steaming
Evaporate, and strictly control the condition of II grade of molecular distillation, the component flowed out along condensation column is the konjak ceramide sample of high-purity
Product.
2. the method that a kind of molecular distillation according to claim 1 isolates and purifies konjak ceramide, it is characterised in that：Institute
State in step 1, konjak ceramide supercritical CO2C in fluid extract6- ceramide content is 10%~20%.
3. the method that a kind of molecular distillation according to claim 1 isolates and purifies konjak ceramide, it is characterised in that：Institute
State in step 1, preheating temperature is 60~80 DEG C.
4. the method that a kind of molecular distillation according to claim 1 isolates and purifies konjak ceramide, it is characterised in that：Institute
State in step 2, I grade of molecule distillation condition is：0.1~10Pa of vacuum, 160~220 DEG C of vapo(u)rizing temperature, charging rate 1~
5ml/min, 0~10 DEG C of condensation temperature, 150~400r/min of knifing rotating speed.
5. the method that a kind of molecular distillation according to claim 1 isolates and purifies konjak ceramide, it is characterised in that：Institute
State in step 3, II molecular distillation condition is：20~100Pa of vacuum, 120~160 DEG C of vapo(u)rizing temperature, charging rate 1~
5ml/min, 10~20 DEG C of condensation temperature, 150~350r/min of knifing rotating speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710999197.8A CN107721871B (en) | 2017-10-20 | 2017-10-20 | Method for separating and purifying konjak ceramide by molecular distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710999197.8A CN107721871B (en) | 2017-10-20 | 2017-10-20 | Method for separating and purifying konjak ceramide by molecular distillation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107721871A true CN107721871A (en) | 2018-02-23 |
| CN107721871B CN107721871B (en) | 2020-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710999197.8A Active CN107721871B (en) | 2017-10-20 | 2017-10-20 | Method for separating and purifying konjak ceramide by molecular distillation |
Country Status (1)
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN104004591A (en) * | 2014-05-22 | 2014-08-27 | 河南三利食品有限公司 | Extraction and purification method of garlic essential oil |
| CN104083556A (en) * | 2014-07-15 | 2014-10-08 | 广州中大南沙科技创新产业园有限公司 | Method for extracting konjak ceramide from konjak |
-
2017
- 2017-10-20 CN CN201710999197.8A patent/CN107721871B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN104004591A (en) * | 2014-05-22 | 2014-08-27 | 河南三利食品有限公司 | Extraction and purification method of garlic essential oil |
| CN104083556A (en) * | 2014-07-15 | 2014-10-08 | 广州中大南沙科技创新产业园有限公司 | Method for extracting konjak ceramide from konjak |
Non-Patent Citations (1)
| Title |
|---|
| 李海池: "超临界CO2萃取分子蒸馏提取分离磨芋神经酰胺", 《中药材》 * |
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| CN107721871B (en) | 2020-10-27 |
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