CN101347419A - Stable state vitamin K3and method of preparing the same - Google Patents
Stable state vitamin K3and method of preparing the same Download PDFInfo
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- CN101347419A CN101347419A CNA200810139659XA CN200810139659A CN101347419A CN 101347419 A CN101347419 A CN 101347419A CN A200810139659X A CNA200810139659X A CN A200810139659XA CN 200810139659 A CN200810139659 A CN 200810139659A CN 101347419 A CN101347419 A CN 101347419A
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- vitamin
- menadione
- stable state
- steady
- sulphuric acid
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Abstract
The invention discloses a vitamin K, in particular a steady-state vitamin K3 and a preparation method thereof. The steady-state vitamin K3 is characterized by being made from the following materials: menadione, sodium metabisulfite, niacinamide and sulphuric acid. The preparation method of the steady-state vitamin K3 comprises the steps as follows: the menadione and alcohol water blend are added to a 500ml reaction bottle, fully stirred and pulped, and then the sodium metabisulfite and the niacinamide are added and continuously stirred to facilitate dissolution, the sulphuric acid is slowly added dropwise, and the pH is regulated to 3-5 to obtain a great amount of white crystals, and the white crystals are filtered, washed and dried to obtain the pure K3 with high steady state. The vitamin K3 has high biological activity and maintains vitamin PP efficiency which is the inherent nutritional function of the niacinamide group in MNB structure, that is, a product has the two functions of vitamin K3 and vitamin PP simultaneously, so the vitamin K3 has higher economical efficiency.
Description
(1) technical field
The present invention relates to a kind of vitamin K, particularly a kind of stable state vitamin K
3And preparation method thereof.
(2) background technology
Vitamin K is the derivant of menadione, has another name called coagulation vitamin or antihemorrhagic vitamin, is to form necessary kind of vitamin of thrombinogen in the animal body.The vitamin K that nature exists has two classes: the phylloquinone that exists in the green plants is called vitamin K
1, another kind of by reaching the synthetic menaquinone of other microorganisms in the animal intestine, be called vitamin K
2Synthetic vitamin K arranged
3, K
4Vitamin K
1Also can manually synthesize.Vitamin K
3Active high, belong to water solublity, easy to use, therefore be most widely used.The major physiological function of vitamin K is to promote the synthetic thrombin of liver and proconvertin, IX X, and plays activation, participates in coagulation process.The animal K that is deficient in vitamin can cause internal hemorrhage, wound cruor time extending or bleed more than.Except that Blood clotting, it is reported that vitamin K dependent protein matter and peptide participate in calcium metabolism.Generally speaking, because the certain micro-organisms of animal alimentary canal can synthesize enough vitamin Ks
2, adults is difficult for lacking.Young animal, particularly cage bird can not be by synthetic vitamin K
2Satisfy the demand, in addition, when intestinal tract disease or animal were taken broad ectrum antibiotic and antibacterial medicine preparation for a long time, the enteric microorganism vigor descended, and can cause vitamin K deficiency; Utilization rate by the dicoumarol reduction vitamin K that forms in the septic plant feed contains this thing and is added with sulfonamides in feedstuff, during antibiotic, need to increase daily ration vitamin K content.Vitamin K is easily destroyed by light and alkali, should keep in Dark Place.
Present China vitamin K
3Main as veterinary drug and feed additive, agricultural and green coating field also belong to blank.On agricultural, can be used as plant growth regulator, some countries in Japan, Russia, Ukraine and Europe have carried out a large amount of work, the domestic application test that also carried out on crops such as vegetable, Oryza sativa L. to this, effect is very obvious, can make increasing crop yield more than 10%.
Veterinary drug and feed additive aspect: vitamin K
3Be the indispensable nutrient of poultry vital movement, be feed additive must add composition.It has unique hemostatic function, can effectively prevent poultry body constitution weakness, subcutaneous and visceral hemorrhage; Can promote animal growth and development, quicken the mineralization of skeleton; The participation poultry embryo forms, and guarantees the young bird survival rate; Also can with the same usefulness of other medicines, diseases such as control coccidiosis, Hakuri and cholera etc. are present vitamin Ks
3Most widely used field.
Human prescription face: it participates in the synthetic of thrombinogen in liver, be one of the most classical hemorrhage, and effects such as antiinflammatory, cough-relieving, analgesia are arranged, can treat diseases such as hepatitis, enteritis, dysentery, aspect the inhibition neoplasm anticancer, the U.S. formally is used for clinical, and effect is remarkable.
The agricultural aspect: as plant growth regulator, promoter, herbicide etc., can make cold-resistant, drought-enduring, anti-lodging, precocity, volume increase such as crops and grain, vegetable, fruit, fundamentally improve fruit quality, and also without any side effects.Application development on Europe, Japanese agriculture is rapid.We cooperate with Anshan suburb farming popularization center, and Oryza sativa L., vegetable etc. has been carried out application test, and effect is remarkable, and its market potential is huge.
Other aspects: with vitamin K
3Being the sapecial coating of main component, can effectively preventing knot extension marine organisms such as steamer, warship, is to substitute the ideal loop friendly coating that Contamination Coatings is arranged at present.
The metabolic characteristic of vitamin K: the vitamin K product on the market is actual to be vitamin K
3Various salts.The vitamin K that domestic animal is taken in
3, can directly be converted into bioactive vitamin K by liver or by enteric microorganism
2, and vitamin K
1Can in liver, accumulate and not change.Synthesizing of the animal body intravascular coagulation factor is the existence that depends on vitamin K.Vitamin K
1With by vitamin K
3The vitamin K that changes into
2, the biological activity that is showed is identical.Vitamin K is fat-soluble, has only vitamin K
3Salt water-soluble.The same with other fatsoluble vitamiies (vitamin A, vitamin D, vitamin E), the lipid of vitamin K in feedstuff is absorbed by body, and it absorbs efficiently, needs the assistance of cholic acid and pancreatic juice.Therefore, any obstacle on the lipid absorption machine Neo-Confucianism all can reduce the activity of vitamin K.The absorption efficiency of vitamin K is because of the difference of dosing method make a variation big (range of variation 10%～70%).Some studies show that: vitamin K
3Almost can be absorbed fully, and vitamin K
1Have only 50% can be absorbed.
The function of vitamin K: vitamin K is the synthetic necessary of many plasma coagulation factorses.The synthetic of thrombinogen (factor II) and plasma coagulation factors VII, IX, X all will depend on vitamin K, if be deficient in vitamin K, the time of blood coagulation just prolongs.Above-mentioned 4 kinds of blood coagulating proteins are the precursor of synthetic non-activity in liver earlier, then by the effect of vitamin K, is converted into the albumen of biologically active.If add vitamin K for the domestic animal that is in the vitamin K deficiency state, low-level thrombin can recover normal activity very soon in 4h.If but do not have the effect of liver, this active recovery would be impossible.The coenzyme (carboxylase) that also has some to depend on vitamin K is relevant with the formation of bone, and bone calcium is because of being to find a kind of protein that depends on vitamin K in bone, and this protein had just taken place when the Embryo Gallus domesticus phase, osseous tissue began the placer deposits material.Also have a kind of enzyme that depends on vitamin K in addition, it participates in the metabolism of calcium in the skin forming process.
Vitamin K deficiency: the cardinal symptom of vitamin K deficiency is that blood coagulation is obstructed, and the thrombinogen level reduces in the blood, thereby causes cruor time extending and hemorrhage.Vitamin K contains quantity not sufficient (adding deficiency or poor stability) in the daily ration, enteral microorganism synthesis capability reduces (use of disulfonamide thing), the incomplete absorption of vitamin K (existence of dicoumarol, coccidiosis or other enteropathogens of antagonist such as coumarin or the generation of going mouldy), perhaps liver metabolism function reduction (mycotoxin or disease cause) can both cause vitamin K deficiency.
The above analysis, vitamin K
3As important a kind of product of vitamin K, it uses more and more, more and more wider.But because common vitamin K
3The character instability, it is rotten to see that light easily decomposes, thereby loses biological activity.
Used vitamin K in present China feedstuff
3(be called menadione sodium bisulfite, MSB) solved partially absorbing property and zest problem, but its stability problem still can't solve, in the time of in being blended in complete feed, the activity of MSB will disappear in several weeks.And the value of vitamin K3 should be estimated by biological activity and the stability program in premix material, from development trend, and stable type VK
3Will progressively replace present MSB.
The process that the applicant adopts in development process mainly contains following several: (one) is raw material with nicotiamide, hydrochloric acid, 25 ℃ react the nicotinoyl amide hydrochloride, with menadione sodium bisulfite (MSB) additive reaction takes place then, the material proportion of reaction is: n (menadione sodium bisulfite): n (nicotiamide): n (hydrochloric acid)=1: 1.2: 1.25, obtain stable vitamin K complex 3 (MNB), yield 95% (in menadione sodium bisulfite).This method is concerning the intermediate menadione of preciousness, and yield has only about 50%, and again nicotiamide of 20% that consumes more, so cost is higher; (2) with menadione sodium bisulfite (MSB): nicotiamide: the sulphuric acid mol ratio is 1: 1: 0.52 synthesizing stable type vitamin K3 (MNB) at normal temperatures.Though the more preceding a kind of method of this method has consumed nicotiamide less, concerning menadione, do not reduce.
(3) summary of the invention
The present invention provides a kind of stable state vitamin K in order to remedy the deficiencies in the prior art
3And preparation method thereof, this stable state vitamin K
3More common attitude has higher stability and biological activity, has reduced the independent addition of nicotiamide in the feedstuff simultaneously again.
The present invention is achieved through the following technical solutions:
A kind of stable state vitamin K
3, its special character is: be to be made by the material of following weight proportion: menadione 100g, sodium pyrosulfite 100～200g, nicotiamide 70～100g, sulphuric acid 40～60 grams.
A kind of stable state vitamin K
3Preparation method, its special character is: 100g menadione, 80% alcohol water blend 300ml are added in the 500ml reaction bulb, abundant stirring to pulp, adding sodium pyrosulfite 100～200g then clarifies to solution in 40～50 ℃ of reactions 2 hours, add 70～100g nicotiamide and continue stirring and dissolving, slowly drip 40～60 gram sulphuric acid then and transfer PH=3～5, a large amount of white crystals, filter, wash, dry the high stable state K3 of pure product.
Stable state vitamin K of the present invention
3Be on the basis of common attitude, in conjunction with the nicotiamide micel, replace sodium ion and three water of crystallization in the common attitude, eliminated the initiation product factors of instability--the existence of-hydrone on the one hand, macromolecular mass has covered the path that isomer transforms on the other hand, suppress the generation of isomer, auxiliary group has conversion and an absorption that is beneficial to vitamin K3 in the organism simultaneously.
The specific activity of MNB of the present invention and MSB is:
The MSB of identical menadione content, MNB sample be sealed under the room temperature store 120 days, the storage rate result is as follows:
| The VK3 source | After 30 days | After 60 days | After 90 days | After 120 days |
| MNB | 97.5％ | 90％ | 85％ | 83％ |
| MSB | 79％ | 61％ | 46％ | 32.5％ |
MNB of the present invention is composited by a part MSB and a part nicotiamide (vitamin PP), because the nicotiamide molecule has replaced Na ion and 3 hydrones on the MSB molecule, can avoid menadione to cause its activity to disappear because of factors such as light, heat, moisture, simultaneously because the existence of auxiliary group also helps the conversion and the absorption of vitamin K3 in the organism, therefore, the biological activity height of this product, keep original the trophic function---vitamin PP effect of nicotiamide group in the MNB structure simultaneously, promptly a kind of product has vitamin K simultaneously
3With two kinds of functions of vitamin PP, so have higher economy.
(4) specific embodiment
Embodiment 1:
With weight proportion: n (menadione): n (sodium pyrosulfite): n (nicotiamide): n (sulphuric acid)=1: 1.5: 0.8: 0.4 synthesizing stable type vitamin K3 (MNB) under certain condition, can be increased to more than 75% to the menadione yield, greatly reduce production cost, have high economic benefit and social benefit.Concrete operations are as follows: 100g (folding hundred) menadione, 80% alcohol water blend 300ml are added in the 500ml reaction bulb, abundant stirring to pulp, adding sodium pyrosulfite (content＞98%) 150g then clarifies to solution in 40-50 ℃ of reaction 2 hours, add 85g nicotiamide (content＞99%) and continue stirring and dissolving, slowly drip sulphuric acid then and transfer PH=3-5, get a large amount of white crystals, filter, wash, dry to such an extent that the high stable state K3 of pure product is 284.6g, yield is 75.6% (to menadione).
Embodiment 2:
This stable state vitamin K
3, be to make: menadione 100g, sodium pyrosulfite 150g, nicotiamide 90g, sulphuric acid 55 grams by the material of following weight proportion.
This stable state vitamin K
3Preparation method as follows: 100g menadione, 80% alcohol water blend 300ml are added in the 500ml reaction bulb, abundant stirring to pulp, adding sodium pyrosulfite 150g then clarifies to solution in 40～50 ℃ of reactions 2 hours, add the 90g nicotiamide and continue stirring and dissolving, slowly Dropwise 55 gram sulphuric acid are transferred PH=3～5 then, get a large amount of white crystals, filter, wash, dry to such an extent that the high stable state K3 of pure product is 285.8g, yield is 76.0%.
Claims (2)
1. stable state vitamin K
3, it is characterized in that: be to make: menadione 100g, sodium pyrosulfite 100～200g, nicotiamide 70～100g, sulphuric acid 40～60 grams by the material of following weight proportion.
2. stable state vitamin K
3Preparation method, it is characterized in that: 100g menadione, 80% alcohol water blend 300ml are added in the 500ml reaction bulb, abundant stirring to pulp, adding sodium pyrosulfite 100～200g then clarifies to solution in 40～50 ℃ of reactions 2 hours, add 70～100g nicotiamide and continue stirring and dissolving, slowly drip 40～60 gram sulphuric acid then and transfer PH=3～5, a large amount of white crystals, filter, wash, dry the high stable state K3 of pure product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810139659XA CN101347419A (en) | 2008-09-02 | 2008-09-02 | Stable state vitamin K3and method of preparing the same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810139659XA CN101347419A (en) | 2008-09-02 | 2008-09-02 | Stable state vitamin K3and method of preparing the same |
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|---|---|
| CN101347419A true CN101347419A (en) | 2009-01-21 |
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|---|---|---|---|
| CNA200810139659XA Pending CN101347419A (en) | 2008-09-02 | 2008-09-02 | Stable state vitamin K3and method of preparing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955217A (en) * | 2010-05-31 | 2011-01-26 | 北京颖新泰康国际贸易有限公司 | Preparation method of menadione nicotinamide bisulfite |
| CN104163779A (en) * | 2014-06-06 | 2014-11-26 | 浙江工业大学 | Method for preparing menadione sodium bisulfite continuously in tubular type reactor |
-
2008
- 2008-09-02 CN CNA200810139659XA patent/CN101347419A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955217A (en) * | 2010-05-31 | 2011-01-26 | 北京颖新泰康国际贸易有限公司 | Preparation method of menadione nicotinamide bisulfite |
| CN101955217B (en) * | 2010-05-31 | 2012-05-09 | 北京颖新泰康国际贸易有限公司 | Preparation method of menadione nicotinamide bisulfite |
| CN104163779A (en) * | 2014-06-06 | 2014-11-26 | 浙江工业大学 | Method for preparing menadione sodium bisulfite continuously in tubular type reactor |
| CN104163779B (en) * | 2014-06-06 | 2016-04-13 | 浙江工业大学 | A kind of pipe type continuously prepares the method for sodium menadione sulfate |
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Open date: 20090121 |