CN1069269A - Extract the method for natural VE from no phenol cotton oil - Google Patents
Extract the method for natural VE from no phenol cotton oil Download PDFInfo
- Publication number
- CN1069269A CN1069269A CN 91105454 CN91105454A CN1069269A CN 1069269 A CN1069269 A CN 1069269A CN 91105454 CN91105454 CN 91105454 CN 91105454 A CN91105454 A CN 91105454A CN 1069269 A CN1069269 A CN 1069269A
- Authority
- CN
- China
- Prior art keywords
- normal hexane
- phase
- mutually
- doubly measures
- cotton oil
- 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.)
- Pending
Links
- 229920000742 Cotton Polymers 0.000 title claims abstract description 16
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000284 extract Substances 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 235000002378 plant sterols Nutrition 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- 238000007127 saponification reaction Methods 0.000 claims abstract description 5
- 238000004821 distillation Methods 0.000 claims abstract description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 229930003427 Vitamin E Natural products 0.000 claims description 13
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 13
- 235000019165 vitamin E Nutrition 0.000 claims description 13
- 229940046009 vitamin E Drugs 0.000 claims description 13
- 239000011709 vitamin E Substances 0.000 claims description 13
- 229960004756 ethanol Drugs 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 235000019154 vitamin C Nutrition 0.000 claims description 4
- 239000011718 vitamin C Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 210000000582 semen Anatomy 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000009874 alkali refining Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 239000002417 nutraceutical Substances 0.000 description 1
- 235000021436 nutraceutical agent Nutrition 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Edible Oils And Fats (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method of extracting natural VE from no phenol cotton oil.Its key step comprises: alcohol extracting, phase-splitting, backflow saponification, n-hexane extraction, washing, freezing and remove precipitation, concentrate distillation etc.The inventive method adopts and extracts with dehydrated alcohol earlier, resaponifying, again with the technology of n-hexane extraction, not only can reduce the consumption of material N aOH and normal hexane greatly, and the purity height of extract, no phenol cotton oil after the extraction is edible still, can also obtain the plant sterol of medical value as byproduct simultaneously.
Description
The present invention relates to a kind of method, belong to the method for making class of the pharmaceutical product that contains organic effective constituent from no phenol cotton oil extraction natural VE.
The vitamin-E of selling on the present market generally adopts chemical process to synthesize and forms, Chinese patent CN88100406A discloses a kind of " extracting nutraceutical methods such as vitamin-E from Semen Maydis oil ", with Semen Maydis oil is raw material, earlier remove free fatty acids and colloid by alkali-refining process, carry out centrifugal molecular distillation then, overhead product after filtration, allotment, pelleting can make a kind of nutritious prod that contains vitamin-E.The shortcoming of this method is that quantity of alkali consumption is bigger, and vitamin-E loses easily, and the content of vitamin-E is lower in the prepared overhead product, and 20～60mg/g is only arranged.
The purpose of this invention is to provide a kind of method, not only save material, and the content of vitamin-E is higher in the extract from no phenol cotton oil extraction natural VE.
The objective of the invention is to reach as follows: a kind of method from no phenol cotton oil extraction natural VE, it comprises the steps:
A, alcohol extracting: a no phenol cotton oil of doubly measuring and a that (80～120) rise that at first add 100 liters in retort doubly measure dehydrated alcohol, reach the anhydrous sodium sulphate that (0.8～1.2) kilogram a doubly measures, boiled 2～5 minutes, and made that contained vitamin-E was dissolved in the dehydrated alcohol in the no phenol cotton oil.Trace water in the adsorbable material of anhydrous sodium sulphate, a are positive count, and all a is same therewith for following a;
B, phase-splitting: employing is left standstill or centrifugal method makes the complete phase-splitting of above-mentioned mixed solution, and the no phenol cotton oil after the phase-splitting is edible still.
C, backflow saponification: the ethanol that obtains after phase-splitting in retort is added to a NaOH that doubly measures and the vitamins C that (0.6～0.8) kilogram a doubly measures of (3～5) kilogram, is heated to boiling, feeds nitrogen simultaneously in reaction solution, refluxes 0.5～2 hour.Vitamins C and nitrogen can prevent the vitamin-E oxidation, the NaOH that is added can make after the phase-splitting ethanol mutually in contained lipid-soluble substance saponification.
D, n-hexane extraction: add normal hexane and (40～60) that a that (80～120) rise doubly measures in mutually to the above-mentioned ethanol that makes and rise the water that a doubly measures, after the stirring, the sealing and standing layering obtains containing the normal hexane phase of vitamin-E;
E, washing: with each mutually the water of the normal hexane that makes, wash 2～4 times, remove water-soluble impurity with 2～3 times of weight.
F, freezing and remove precipitation: mutually freezing 12～48 hours of the normal hexane after will washing, temperature is-5 °～-15 ℃, makes the wherein contained saponified plant sterol that is difficult for form precipitation at low temperatures, then precipitate and separate is gone out.
G, concentrated distillation: distill the above-mentioned normal hexane phase that makes, the distillment that obtains is the enriched material of natural VE.
Comparison prior art of the present invention has following advantage:
1, with contained vitamin-E in the no phenol cotton oil of dehydrated alcohol extraction, the no phenol cotton oil after the extraction is edible still, thereby has reduced production cost earlier in the present invention.
2, with after the dehydrated alcohol extraction, to ethanol mutually in adding NaoH carry out saponification, so just greatly reduce the consumption of NaOH, reduced cost.
3, earlier with the dehydrated alcohol extraction, use n-hexane extraction again, both can reduce the consumption of normal hexane, help removing the fat of higher fatty acid contained in the starting material and alcohol formation again, improved the purity of finished product greatly.
4, after n-hexane extraction, washing, the plant sterol precipitation that obtains after freezing proves a kind of good natural drug that reduces body's cholesterol through modern medicine, thereby has further improved economic benefit of the present invention and social benefit.
The present invention will be further described as follows in conjunction with the embodiments:
At first in retort, add 100 liters of no phenol cotton oils and 100 liters of dehydrated alcohols, and add 1 kilogram of anhydrous sodium sulphate, boiled 2～5 minutes, in tophan pot, carry out phase-splitting then, speed of rotation is 500～1000 rev/mins, and centrifugal 20 minutes, the oil phase that obtains is edible still.The ethanol that obtains is introduced the retort that has reflux condensing tube mutually, add 4 kilograms of NaOH and 0.7 kilogram of vitamins C, and feed nitrogen in mutually, be heated to boiling, and refluxed 1.5 hours to ethanol.Again ethanol is introduced tophan pot mutually, and add 100 liters of normal hexanes and 50 premium on currency, after the stirring, sealing and standing, treat ethanol mutually with normal hexane mutually after the layering, normal hexane is fed band end opening retort mutually, the water that adds 2 times of amounts, washing twice, with mutually freezing 24 hours of normal hexane after the washing, temperature is-10 ℃, feed the sealing tophan pot again, the precipitate and separate that plant sterol under the low temperature forms is gone out, the normal hexane that obtains is introduced distiller mutually distill, the overhead product that obtains is natural vitamin E concentrate.Experiment shows, uses the inventive method to extract wherein contained natural VE from no phenol cotton oil, and the rate of recovery can reach more than 70%, and content of vitamin E reaches about 40% in the extract that makes.
Claims (1)
1, a kind of method from no phenol cotton oil extraction natural VE is characterized in that it comprises the steps:
A, alcohol extracting: add a that no phenol cotton oil that 100 liters a doubly measures and (80～120) rise and doubly measure dehydrated alcohol in retort, and add the anhydrous sodium sulphate that (0.8～1.2) kilogram a doubly measures, boiled 2～3 minutes, a is a positive count, following a all therewith a with;
B, phase-splitting: adopt and to leave standstill or centrifugal method makes the complete phase-splitting of above-mentioned mixed solution, obtain oil phase and ethanol respectively mutually;
C, backflow saponification: the ethanol that obtains after phase-splitting in retort is added to a NaOH that doubly measures and the vitamins C that (0.6～0.8) kilogram a doubly measures of (3～5) kilogram, is heated to boiling, feeds nitrogen simultaneously in reaction solution, refluxes 0.5～2 hour;
The extraction of D, normal hexane: add the normal hexane that a that (80～120) rise doubly measures in mutually to the above-mentioned ethanol that makes and rise the water that a doubly measures with (40～60), after the stirring, the sealing and standing layering obtains containing the normal hexane phase of vitamin-E;
E, washing:, wash 2～4 times with each mutually the water of the normal hexane that makes with 2～3 times of weight;
F, freezing and remove precipitation: mutually freezing 12～48 hours of the normal hexane after will washing, temperature are-5 °～-15 ℃, then the plant sterol precipitate and separate of freezing formation are gone out;
G, concentrated distillation: distill the above-mentioned normal hexane phase that makes, the distillment that obtains is the enriched material of natural VE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91105454 CN1069269A (en) | 1991-08-12 | 1991-08-12 | Extract the method for natural VE from no phenol cotton oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91105454 CN1069269A (en) | 1991-08-12 | 1991-08-12 | Extract the method for natural VE from no phenol cotton oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1069269A true CN1069269A (en) | 1993-02-24 |
Family
ID=4907165
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91105454 Pending CN1069269A (en) | 1991-08-12 | 1991-08-12 | Extract the method for natural VE from no phenol cotton oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1069269A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094935C (en) * | 1998-12-24 | 2002-11-27 | 中国科学院长春应用化学研究所 | Process for extracting natural VE from sunflower seed oil |
| CN103467431A (en) * | 2013-09-06 | 2013-12-25 | 中国农业科学院棉花研究所 | Method for extracting vitamin E from cottonseed oil |
| CN111454243A (en) * | 2020-04-08 | 2020-07-28 | 河北圣奥化妆品有限公司 | Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E |
| US12370585B2 (en) | 2019-09-06 | 2025-07-29 | Arkema France | Method for recovering and separating unsaturated fluorinated hydrocarbons |
-
1991
- 1991-08-12 CN CN 91105454 patent/CN1069269A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094935C (en) * | 1998-12-24 | 2002-11-27 | 中国科学院长春应用化学研究所 | Process for extracting natural VE from sunflower seed oil |
| CN103467431A (en) * | 2013-09-06 | 2013-12-25 | 中国农业科学院棉花研究所 | Method for extracting vitamin E from cottonseed oil |
| WO2015032166A1 (en) * | 2013-09-06 | 2015-03-12 | 中国农业科学院棉花研究所 | Method for extracting vitamin e from cottonseed oil |
| US12370585B2 (en) | 2019-09-06 | 2025-07-29 | Arkema France | Method for recovering and separating unsaturated fluorinated hydrocarbons |
| CN111454243A (en) * | 2020-04-08 | 2020-07-28 | 河北圣奥化妆品有限公司 | Ultrasonic grinding-high pressure homogenate grading wall breaking extraction method of cucumber vitamin E |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |