CN105906590B - A kind of preparation method for mending iron medicine - Google Patents
A kind of preparation method for mending iron medicine Download PDFInfo
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- CN105906590B CN105906590B CN201610271313.XA CN201610271313A CN105906590B CN 105906590 B CN105906590 B CN 105906590B CN 201610271313 A CN201610271313 A CN 201610271313A CN 105906590 B CN105906590 B CN 105906590B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of preparation method for mending iron medicine, specifically a kind of preparation technology of L ferrous ascorbates, including preparing rough L ferrous ascorbates as raw material with food-grade ferrous carbonate, high-purity reduced iron powder, L ascorbic acid, and it is refined by EDTA, activated carbon and ethanol, obtain pharmaceutical grade supplemental iron compound --- L ferrous ascorbates.
Description
Technical field
The invention belongs to field of medicaments, and in particular to a kind of ferrous preparation technology of L-AA.
Technical background
L-AA is ferrous not only to have the nutritional characteristic of L-AA and ferrous salt, but also compensate for both
Some shortcomings, and be provided with some it is new the characteristics of.L-AA ferrous iron has preferably anti-oxidant than L-AA
Property, and it is smaller than the side effect of L-AA；Relative to general ferrous salt, resist as the L- in third generation ferrous-fortifier
Bad hematic acid is ferrous, it is easier to which be absorbed by the body utilization, toxic and side effect also very little, with very extensive market prospects.In food row
In industry, L-AA ferrous iron can be as the antioxidant of food, hardening agent and additive etc.；In pharmaceuticals industry, L- is anti-bad
Hematic acid is ferrous to have L-AA and the equal pharmacological action containing ferrous medicine, for treat L-AA deficiency disease and
Prophylactic treatment iron deficiency, and be easily absorbed by the body after L-AA is made ferrous salt, stability enhancing.
CherbourgP.Rao et al. was once reacted using L-AA and frerrous chloride in 1999 in methanol solution
Synthesize L-AA ferrous, yield only had 42%-58% at that time, and through the content ratio of Instrument measuring Fe (ll) and Fe (III)
It is 1:2, it can thus be appreciated that ferrous content is less in product.The conjunction ferrous it is therefore desirable to seek a kind of new L-AA
Into method.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art, design a kind of a kind of L- for being directed to medical industry production
The preparation technology of ferrous ascorbate.To solve this problem, can carry out by the following method.
A kind of ferrous preparation technology of L-AA, comprises the following steps：
1）By food-grade ferrous carbonate and high-purity reduced iron powder by ratio of weight and the number of copies 10:The ratio of 1-1.5 is well mixed；
2）Dissolved in the purified water for adding through ultrasound degassing by the L-AA of 12-15 parts of weight, and by step 1）In
Mixture add L-AA solution in heat and be slowly stirred 2-3 hours；
3）By step 2）In reaction system through 0.22 μm of membrane filtration, collect filtrate；
4）To step 3）Add EDTA to be slowly stirred 20-40min, add the millesimal activated carbon of ferrous carbonate weight,
Stir holding 5-10 minutes, through 0.22 μm of membrane filtration, collects filtrate；
5）To absolute ethyl alcohol is added in filtrate, 10-15 hours is stood at 0-5 DEG C, treat that purple crystals are separated out and finish, taken out
Filter, and use absolute ethanol washing.
6）It is vacuum dried at 35-45 DEG C and is obtained final product for 4-6 hours.
Wherein step 2）, preferably heating-up temperature is 40-50 DEG C, step 4）Middle EDTA additions are ferrous carbonate weight
0.1%-1%, preferably 0.3%.
Specific embodiment
Come to be described further present invention by the following examples.
Embodiment 1：
Weigh 120g L-AAs and be dissolved in the purified water of 300g ultrasound degassings, by 100g food-grade ferrous carbonates
It is added in L-AA solution after being mixed in proportion with the high-purity reduced iron powders of 15g, is heated to 45 DEG C, is slowly stirred
2h, by reaction system through 0.22 μm of filter membrane suction filtration, the EDTA to addition 0.3g in the filtrate collected continues to be slowly stirred 30min,
0.1g activated carbons are added, is stirred, keep 10min, through 0.22 μm of filter membrane suction filtration, collect filtrate, to adding 600g in filtrate
Absolute ethyl alcohol, system temperature is reduced to 4 DEG C, stand 15h, treat that purple crystals are separated out and finish, through 0.22 μm of filter membrane suction filtration, be used in combination
Absolute ethanol washing 2 times.Filter cake is vacuum dried 4 hours at 45 DEG C and is obtained final product.
The ferrous yield of L-AA is 94.2% after testing, and purity is 99.3%.
Embodiment 2：
Weigh 120kg L-AAs and be dissolved in the purified water of 300kg ultrasound degassings, 100kg food-grades carbonic acid is sub-
Iron and the high-purity reduced iron powders of 12kg are added in L-AA solution after mixing in proportion, and are heated to 40 DEG C, are slowly stirred
2h is mixed, by reaction system through 0.22 μm of filter membrane suction filtration, continues to be slowly stirred to the EDTA of 0.3kg is added in the filtrate collected
30min, adds 0.1kg activated carbons, stirs, and keeps 10min, through 0.22 μm of filter membrane suction filtration, filtrate is collected, in filtrate
The absolute ethyl alcohol of 600kg is added, system temperature is reduced to 4 DEG C, stand 15h, treated that purple crystals are separated out and finish, through 0.22 μm of filter membrane
Suction filtration, and with absolute ethanol washing 2 times.Filter cake is vacuum dried 4 hours at 45 DEG C and is obtained final product.
The ferrous yield of L-AA is 85.6% after testing, and purity is 99.0%.
Embodiment 3：
Weigh 150kg L-AAs and be dissolved in the purified water of 400kg ultrasound degassings, 100kg food-grades carbonic acid is sub-
Iron and the high-purity reduced iron powders of 15kg are added in L-AA solution after mixing in proportion, and are heated to 40 DEG C, are slowly stirred
3h is mixed, by reaction system through 0.22 μm of filter membrane suction filtration, continues to be slowly stirred to the EDTA of 0.3kg is added in the filtrate collected
30min, adds 0.1kg activated carbons, stirs, and keeps 10min, through 0.22 μm of filter membrane suction filtration, filtrate is collected, in filtrate
The absolute ethyl alcohol of 800kg is added, system temperature is reduced to 5 DEG C, stand 12h, treated that purple crystals are separated out and finish, through 0.22 μm of filter membrane
Suction filtration, and with absolute ethanol washing 2 times.Filter cake is vacuum dried 6 hours at 40 DEG C and is obtained final product.
The ferrous yield of L-AA is 84.5% after testing, and purity is 99.2%.
Embodiment 4：
Weigh 130kg L-AAs and be dissolved in the purified water of 400kg ultrasound degassings, 100kg food-grades carbonic acid is sub-
Iron and the high-purity reduced iron powders of 13kg are added in L-AA solution after mixing in proportion, and are heated to 42 DEG C, are slowly stirred
2.5h is mixed, by reaction system through 0.22 μm of filter membrane suction filtration, continues to be slowly stirred to the EDTA of 0.3kg is added in the filtrate collected
30min, adds 0.1kg activated carbons, stirs, and keeps 10min, through 0.22 μm of filter membrane suction filtration, filtrate is collected, in filtrate
The absolute ethyl alcohol of 800kg is added, system temperature is reduced to 5 DEG C, stand 12h, treated that purple crystals are separated out and finish, through 0.22 μm of filter membrane
Suction filtration, and with absolute ethanol washing 2 times.Filter cake is vacuum dried 6 hours at 40 DEG C and is obtained final product.
The ferrous yield of L-AA is 89.1 % after testing, and purity is 99.1%.
Embodiment 5：
Weigh 120g L-AAs and be dissolved in the purified water of 300g ultrasound degassings, by 100g food-grade ferrous carbonates
It is added in L-AA solution after being mixed in proportion with the high-purity reduced iron powders of 15g, is heated to 45 DEG C, is slowly stirred
2h, by reaction system through 0.22 μm of filter membrane suction filtration, to 0.1g activated carbons are added in the filtrate collected, stirs, and keeps
10min, through 0.22 μm of filter membrane suction filtration, collects filtrate, to the absolute ethyl alcohol that 600g is added in filtrate, system temperature is reduced into 4 DEG C,
15h is stood, is treated that purple crystals are separated out and is finished, through 0.22 μm of filter membrane suction filtration, and with absolute ethanol washing 2 times.By filter cake at 45 DEG C
Lower vacuum drying is obtained final product for 4 hours.
The ferrous yield of L-AA is 69.2% after testing, and purity is 99.3%.
Embodiment 6：
Weigh 120g L-AAs and be dissolved in the purified water of 300g ultrasound degassings, by 100g food-grade ferrous carbonates
It is added in L-AA solution after being mixed in proportion with the high-purity reduced iron powders of 15g, is heated to 80 DEG C, is slowly stirred
2h, by reaction system through 0.22 μm of filter membrane suction filtration, the EDTA to addition 0.3g in the filtrate collected continues to be slowly stirred 30min,
0.1g activated carbons are added, is stirred, keep 10min, through 0.22 μm of filter membrane suction filtration, collect filtrate, to adding 600g in filtrate
Absolute ethyl alcohol, system temperature is reduced to 4 DEG C, stand 15h, treat that purple crystals are separated out and finish, through 0.22 μm of filter membrane suction filtration, be used in combination
Absolute ethanol washing 2 times.Filter cake is vacuum dried 4 hours at 45 DEG C and is obtained final product.
The ferrous yield of L-AA is 80.2% after testing, and purity is 80.3%.
Claims (3)
1. a kind of process of preparing for mending iron medicine, comprises the following steps：
1) by food-grade ferrous carbonate and high-purity reduced iron powder by ratio of weight and the number of copies 10:The ratio of 1-1.5 is well mixed；
2) dissolved in the purified water for adding through ultrasound degassing by the L-AA of 12-15 parts of weight, and by step 1) in it is mixed
Heat and be slowly stirred 2-3 hours in compound addition L-AA solution；
3) by step 2) in reaction system through 0.22 μm of membrane filtration, collect filtrate；
4) to step 3) add EDTA to be slowly stirred 20-40min, add the millesimal activated carbon of ferrous carbonate weight, stirring
It is uniform to be kept for 5-10 minutes, through 0.22 μm of membrane filtration, collect filtrate；
5) to absolute ethyl alcohol is added in filtrate, 10-15 hours is stood at 0-5 DEG C, treats that purple crystals are separated out and finish, suction filtration, and
Use absolute ethanol washing；
6) it is vacuum dried 4-6 hours at 35-45 DEG C.
2. a kind of process of preparing for mending iron medicine as claimed in claim 1, it is characterised in that：Wherein step 2) heating
Temperature is 40-50 DEG C.
3. a kind of process of preparing for mending iron medicine as claimed in claim 1, it is characterised in that：Step 4) in EDTA add
It is the 0.1%-1% of ferrous carbonate weight to measure.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610271313.XA CN105906590B (en) | 2016-04-28 | 2016-04-28 | A kind of preparation method for mending iron medicine |
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| CN201610271313.XA CN105906590B (en) | 2016-04-28 | 2016-04-28 | A kind of preparation method for mending iron medicine |
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