CN108085424A - A kind of preparation method of medical cane sugar - Google Patents
A kind of preparation method of medical cane sugar Download PDFInfo
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- CN108085424A CN108085424A CN201711471850.XA CN201711471850A CN108085424A CN 108085424 A CN108085424 A CN 108085424A CN 201711471850 A CN201711471850 A CN 201711471850A CN 108085424 A CN108085424 A CN 108085424A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/04—Disaccharides
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/005—Purification of sugar juices using chemicals not provided for in groups C13B20/02 - C13B20/14
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
- C13B20/123—Inorganic agents, e.g. active carbon
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/002—Evaporating or boiling sugar juice
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/02—Crystallisation; Crystallising apparatus
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicinal Preparation (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of preparation method of medical cane sugar, using in aqueous phase system, the method crystallized by the way that concentration Temperature fall is complexed prepares medical cane sugar, on the premise of product quality and yield is ensured, simplify operating procedure, it avoids ion exchange process and generates substantial amounts of acidic and alkaline waste water, realize the environmentally protective of production process；Addition of the production process without poisonous and harmful solvent, does not detect residual solvent, and the magma filtrate after filtering can continue to be back to the production of next group, reaches and improves production efficiency and reduction production cost.Present invention process is stable, easy to operate, mild condition, the yield of product and purity are high, obtains product satisfaction《European Pharmacopoeia》8.0 editions requirements to medical cane sugar are suitble to industrialized production, have a good application prospect.
Description
Technical field
The present invention relates to sucrose, and in particular to a kind of preparation method of medical cane sugar.
Background technology
Sucrose, English name：Sucrose, chemical name：Sucrose, molecular formula
For C12H22O11, molecular weight：342.30.Sucrose is colourless crystallization or the bulky powder of white crystalline；It is odorless, it is sweet, in water
In easily dissolve, slightly soluble, almost insoluble in absolute ethyl alcohol in ethanol.Sucrose structural formula is as follows：
Effect of the medicament-grade cane sugar (medical cane sugar) in medical industry for drug seasoning, increases mainly as pharmaceutic adjuvant
Add medicine stability or provide energy etc. for human body.Most important function is to make corrigent or/and tax to medical cane sugar in a medicament
Shape agent, such as 50%~70% syrup make the binder of wet granulation, filler or/and sweet tea as chewable tablets or/and tincture
Taste agent；Or as the corrigent for being used as liquid preparation for oral administration containing 85% syrup or armaticity syrup.
It is more and more stringenter to the quality criteria requirements of preparation in terms of the external pharmaceutical drugs of recent year and medicine management,
There is stringent regulation to the uniformity of drug and pharmaceutic adjuvant content, stability, toxic side effect, bioavilability.Common food
Grade sucrose is since the content of its impurity is higher, and particularly metal ion therein, sulphite and reduced sugar etc. can influence
The quality of drug and shorten its shelf-life, and bring harm to drug safety.Therefore, food grade sucrose does not adapt to medicine
Object produces the requirement to pharmaceutic adjuvant.And medicament-grade cane sugar is since purity is high, impurity is few, be effective to ensure that drug quality and
Drug safety.
The researchs such as Wang Lisheng are reported using food grade sucrose as raw material, and legal system is recrystallized using activated carbon decolorizing, alcohol-water
Standby medicament-grade cane sugar；Using alcohol-water as recrystallization system in this method, the amount of ethyl alcohol reaches 80%, and consumption is larger, greatly
The big production cost for improving medical cane sugar.Rainbow etc., which is reported, to carry out sucrose by macroporous absorbent resin to prepare medicine
Use sucrose；This method is related to the pre-treatment and resin regeneration of macroporous absorbent resin, which can generate substantial amounts of soda acid and give up
Water, the post processing of acidic and alkaline waste water not only damages to environment, but also considerably increases production cost and processing cost.Patent
CN101255177A reports a kind of method that ionic exchange fibre technology prepares medicament-grade cane sugar, by food grade sucrose by weight
It is 1 to measure volume ratio:1-100 is dissolved in deionized water, crosses cation exchange fibre, flow velocity 1d-10d/sec., and cation is handed over
It is 1 that fiber, which is changed, with sucrose weight ratio:1-1000；After anion-exchange fibre, flow velocity 1d-10d/sec., anion exchange
The weight ratio of fiber and sucrose is 1:1-1000 is concentrated under reduced pressure into the 10%-40% of water content, and crystallization obtains finished product；This method
The consumption of middle cation and anion exchange fiber is relatively large, and the front and rear processing of exchange fiber easily forms a large amount of acidic and alkaline waste waters, unfavorable
In environmental protection.
The content of the invention
In order to solve the problems in the prior art, it is an object of the invention to provide a kind of preparation method of medical cane sugar,
On the premise of product quality and yield is ensured, operating procedure is simplified, ion exchange process is avoided and generates substantial amounts of soda acid
Waste water, production process are environmentally protective；Addition of the production process without poisonous and harmful solvent simultaneously, magma filtrate after filtering can be with
Continue to be back to the production of next group, improve production efficiency, reduce production cost.
Unless otherwise specified, number of the present invention is parts by weight, and the percentage is mass percent.
The object of the present invention is achieved like this：
The preparation method of medical cane sugar of the present invention, comprises the following steps：Food grade sucrose is added in distilled water, 70
~85 DEG C of speed heating stirring and dissolvings with 30r/min~60r/min；Then add in edible sucrose addition 0.004%~
0.006% EDTA adds activated carbon decolorizing, filters while hot；It is about original that water yield volume is concentrated under reduced pressure at 55~65 DEG C
Volume 85%~90% adds in the crystal seed of edible sucrose addition 0.02%~0.04% into concentrate, in 55~65 DEG C of temperature
The r/min stirring 1~4h of growing the grain of the lower 15r/min of degree~25, add distilled water stirring and dissolving, it is to be dissolved uniformly after depressurize again it is dense
Contracting, is repeated 3 times；Then mechanical agitation Temperature fall crystallize, press filtration, be dried in vacuo at 55~65 DEG C both it is of the invention
Medical cane sugar.
Further, activated carbon of the present invention be injection active carbon, addition for edible sucrose addition 0.04%~
0.06%.
Further, the mixing speed of mechanical agitation Temperature fall of the present invention crystallization is not above 20r/min,
Crystallization time is 6~12h.
Specifically, the preparation method of medical cane sugar of the present invention, comprises the following steps：Food grade sucrose is added in and is distilled
In water, in 70~85 DEG C of speed heating stirring and dissolvings with 30r/min~60r/min；Then edible sucrose addition is added in
0.005% EDTA adds activated carbon decolorizing, filters while hot；The activated carbon is injection active carbon, and addition is edible
Sucrose addition 0.05%；It is about original volume 85%~90% that water yield volume is concentrated under reduced pressure at 55~65 DEG C, to concentrate
The middle crystal seed for adding in edible sucrose addition 0.03%, at a temperature of 55~65 DEG C 15r/min~25r/min stir growing the grain 1~
4h, adds distilled water stirring and dissolving, it is to be dissolved uniformly after be concentrated under reduced pressure again, be repeated 3 times；Then mechanical agitation is natural
Decrease temperature crystalline, for mixing speed not above 20r/min, crystallization time is 6~12h；In 0.01~0.03Mpa press filtrations, 55~65
Be dried in vacuo at DEG C both medical cane sugar of the present invention.
Advantageous effect：
The present invention provides a kind of preparation method of medical cane sugar, by complexing-concentration-drop naturally in aqueous phase system
The method of temperature crystallization prepares medical cane sugar, on the premise of product quality and yield is ensured, simplifies operating procedure, avoids
Ion exchange process generates substantial amounts of acidic and alkaline waste water, and production process is environmentally protective；Production process adds without poisonous and harmful solvent
Add, do not detect residual solvent, the magma filtrate after filtering can continue to be back to the production of next group, not only increase production
Efficiency also reduces production cost.The method of the present invention prepare medical cane sugar crystallization time is short, high income, good product quality, sugarcane
Sugar juice electrical conductivity is less than 15 μ Sm-1, product quality satisfaction《European Pharmacopoeia》Requirements of the EP8.0 to medical cane sugar.The present invention
Middle use water is as solvent, and crystallization condition is relatively mild, and crystallization time is controlled when 6~12 is small or so, preparation system green ring
It protects, product quality is high, crystallization yield more than 90%, and product purity is more than 99%, and crystallographic particle is uniform, and glossiness is good, nothing
Excessively complicated manual operation is needed, production efficiency is high, is suitble to industrialized production.
Specific embodiment
The present invention is specifically described below by specific embodiment, it is pointed out here that following embodiment is served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, the person skilled in the art of this field can be with
Some nonessential modifications and adaptations are made to the present invention according to foregoing invention content.All raw materials of the present invention and reagent are
Commercial product.
Embodiment 1：
750g food grade sucroses are added in 1.5L distilled water, are warming up to 80 DEG C of speed with the r/min of 30r/min~40
Stirring and dissolving；0.0375g EDTA are added in, 0.375g injection active carbons decoloration 30min is added, filters while hot.At 60 DEG C
It is about original volume 85% to be concentrated under reduced pressure into water yield volume, 7.5g crystal seeds is added in into concentrate, with 15r/ at a temperature of 60 DEG C
Min~20r/min stirs growing the grain 1h, during substantial amounts of fine particles to appear, adds 10ml distilled water stirring and dissolvings, treats molten
It is concentrated under reduced pressure again after solution is uniform, is repeated 3 times and more bulky grain crystal occur；Then control machinery mixing speed is 10r/
Min, Temperature fall crystallization 8h, is dried in vacuo at 0.01~0.03Mpa press filtrations, 60 DEG C and obtains medical cane sugar, obtain
65.75g；Yield：87.3%, purity：99.2%.
Reference《European Pharmacopoeia》The detection method of EP8.0 medical cane sugars, medical cane sugar prepared by detection embodiment 1, detection
As a result such as the following table 1.
Medical cane sugar testing result prepared by 1 embodiment 1 of table
| Testing index | Quality standard |
| Appearance | White crystalline powder or colourless glossiness crystal |
| The color of solution | Clarification |
| Electrical conductivity | 12.6μS·m-1 |
| Specific rotation | + 66.3~67.0 |
| Color value | ≤45 |
| Reduced sugar | ≤ 0.1% |
| Sulfate | ≤10ppm |
| Loss on drying | ≤0.1 |
| Bacterial endotoxin | ≤0.25UI/mg |
From the point of view of 1 testing result of table, medical cane sugar prepared by embodiment 1 meets《European Pharmacopoeia》EP8.0 medical cane sugars
Quality criteria requirements.
Embodiment 2：
1000g food grade sucroses are added in 3.0L distilled water, are warming up to 70 DEG C of speed with the r/min of 40r/min~50
Stirring and dissolving；0.05g EDTA are added in, 0.5g injection active carbons decoloration 30min is added, filters while hot.It is depressurized at 60 DEG C
It is about original volume 88% to be concentrated into water yield volume, into concentrate add in 10g crystal seeds, at a temperature of 60 DEG C with 20r/min~
25r/min stirs growing the grain 2h, during substantial amounts of fine particles to appear, adds 13ml distilled water stirring and dissolvings, it is to be dissolved uniformly
It is concentrated under reduced pressure again afterwards, is repeated 3 times and more bulky grain crystal occur；Then control machinery mixing speed is 15r/min, from
Right decrease temperature crystalline 10h is dried in vacuo at 0.01~0.03Mpa press filtrations, 60 DEG C and obtains medical cane sugar, obtains 898g；Yield：
89.8%, purity 99.2%.
With reference to the detection method of embodiment 1, the medical cane sugar of the detection preparation of embodiment 2, testing result such as the following table 2.
Medical cane sugar testing result prepared by 2 embodiment 2 of table
From the point of view of 2 testing result of table, medical cane sugar prepared by embodiment 2 meets《European Pharmacopoeia》EP8.0 medical cane sugars
Quality criteria requirements.
Embodiment 3：
1350g food grade sucroses are added in 5.4L distilled water, are warming up to 85 DEG C of speed with the r/min of 35r/min~45
Stirring and dissolving；0.0675g EDTA are added in, 0.675g injection active carbons decoloration 30min is added, filters while hot.At 60 DEG C
It is about original volume 90% to be concentrated under reduced pressure into water yield volume, into concentrate add in 13.5g crystal seeds, at a temperature of 60 DEG C with
15r/min~20r/min stirs growing the grain 3h, during substantial amounts of fine particles to appear, adds 18ml distilled water stirring and dissolvings,
It is to be dissolved uniformly after be concentrated under reduced pressure again, be repeated 3 times and more bulky grain crystal occur；Then control machinery mixing speed is
12r/min, Temperature fall crystallization 12h, is dried in vacuo at 0.01~0.03Mpa press filtrations, 65 DEG C and obtains medical cane sugar, obtain
1200g；Yield：88.9%, purity 99.4%.
With reference to the detection method of embodiment 1, the medical cane sugar of the detection preparation of embodiment 3, testing result such as the following table 3.
Medical cane sugar testing result prepared by 3 embodiment 3 of table
| Testing index | Quality standard |
| Appearance | White crystalline powder or colourless glossiness crystal |
| The color of solution | Clarification |
| Electrical conductivity | 11.6μS·m-1 |
| Specific rotation | + 66.3~67.0 |
| Color value | ≤45 |
| Reduced sugar | ≤ 0.1% |
| Sulfate | ≤10ppm |
| Loss on drying | ≤0.1 |
| Bacterial endotoxin | ≤0.25UI/mg |
From the point of view of 3 testing result of table, medical cane sugar prepared by embodiment 3 meets《European Pharmacopoeia》EP8.0 medical cane sugars
Quality criteria requirements.
Embodiment 4：
900g food grade sucroses are added in 2.25L distilled water, are warming up to 75 DEG C of speed with the r/min of 30r/min~60
Stirring and dissolving；0.045g EDTA are added in, 0.45g injection active carbons decoloration 30min is added, filters while hot；Subtract at 60 DEG C
It is about original volume 88% that pressure, which is concentrated into water yield volume, 9g crystal seeds is added in into concentrate, with 15r/min at a temperature of 60 DEG C
~25r/min stirs growing the grain 4h, during substantial amounts of fine particles to appear, adds 12ml distilled water stirring and dissolvings, it is to be dissolved
It is concentrated under reduced pressure again after even, is repeated 3 times and more bulky grain crystal occur；Then control machinery mixing speed is 18r/min,
Temperature fall crystallizes 6h, is dried in vacuo at 0.01~0.03Mpa press filtrations, 55 DEG C and obtains medical cane sugar, obtains 779g；Yield：
86.5%, purity 99.0%.
With reference to the detection method of embodiment 1, the medical cane sugar of the detection preparation of embodiment 4, testing result such as the following table 4.
Medical cane sugar testing result prepared by 4 embodiment 4 of table
| Testing index | Quality standard |
| Appearance | White crystalline powder or colourless glossiness crystal |
| The color of solution | Clarification |
| Electrical conductivity | 14.1μS·m-1 |
| Specific rotation | + 66.3~67.0 |
| Color value | ≤45 |
| Reduced sugar | ≤ 0.1% |
| Sulfate | ≤10ppm |
| Loss on drying | ≤0.1 |
| Bacterial endotoxin | ≤0.25UI/mg |
From the point of view of 4 testing result of table, medical cane sugar prepared by embodiment 4 meets《European Pharmacopoeia》EP8.0 medical cane sugars
Quality criteria requirements.
Claims (4)
1. a kind of preparation method of medical cane sugar, comprises the following steps：Food grade sucrose is added in distilled water, 70~85oC
It is heated up stirring and dissolving with the speed of the r/min of 30r/min~60；Then edible sucrose addition 0.004%~0.006% is added in
EDTA adds activated carbon decolorizing, filters while hot；55~65oBe concentrated under reduced pressure under C water yield volume be about original volume 85%~
90%, the crystal seed of edible sucrose addition 0.02%~0.04% is added in into concentrate, in 55~65o15r/min at a temperature of C~
25 r/min stir 1~4h of growing the grain, add distilled water stirring and dissolving, it is to be dissolved uniformly after be concentrated under reduced pressure again, be repeated 3
It is secondary；Then mechanical agitation Temperature fall crystallizes, press filtration, in 55~65oIt is dried in vacuo under C and both obtained.
2. the preparation method of medical cane sugar as described in claim 1, it is characterised in that：The activated carbon is injection active carbon, is added
Enter amount for edible sucrose addition 0.04%~0.06%.
3. the preparation method of medical cane sugar as claimed in claim 1 or 2, it is characterised in that：The mechanical agitation Temperature fall
For the mixing speed of crystallization not above 20r/min, crystallization time is 6~12h.
4. a kind of preparation method of medical cane sugar, comprises the following steps：Food grade sucrose is added in distilled water, 70~85oC
It is heated up stirring and dissolving with the speed of the r/min of 30r/min~60；Then the EDTA of edible sucrose addition 0.005% is added in, then is added
Enter activated carbon decolorizing, filter while hot；The activated carbon is injection active carbon, and addition is edible sucrose addition 0.05%；55~
65oIt is about original volume 85%~90% that water yield volume is concentrated under reduced pressure under C, and edible sucrose addition is added in into concentrate
0.03% crystal seed, in 55~65oThe r/min stirring 1~4h of growing the grain of 15r/min at a temperature of C~25, it is molten to add distilled water stirring
Solution, it is to be dissolved uniformly after be concentrated under reduced pressure again, be repeated 3 times；Then mechanical agitation Temperature fall crystallizes, and mixing speed cannot be high
In 20r/min, crystallization time is 6~12h；In 0.01~0.03Mpa press filtrations, 55~65oIt is dried in vacuo under C and both obtained.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711471850.XA CN108085424A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of medical cane sugar |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110656206A (en) * | 2019-09-24 | 2020-01-07 | 湖南新绿方药业有限公司 | Novel sucrose refining method capable of controlling granularity |
| CN113956302A (en) * | 2021-11-15 | 2022-01-21 | 天津信诚康达药业有限公司 | Recrystallization method of medicinal sucrose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508707A (en) * | 2009-03-25 | 2009-08-19 | 湖南尔康制药有限公司 | Production process for medicinal sucrose |
| CN102351917A (en) * | 2011-09-14 | 2012-02-15 | 北京科技大学 | Method for extracting raffinose from cotton seed meal |
| CN102816192A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Production technology of high-purity stevioside |
| CN105153245A (en) * | 2015-09-23 | 2015-12-16 | 河南正弘药用辅料有限公司 | Production technology for medicinal cane sugar |
-
2017
- 2017-12-29 CN CN201711471850.XA patent/CN108085424A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508707A (en) * | 2009-03-25 | 2009-08-19 | 湖南尔康制药有限公司 | Production process for medicinal sucrose |
| CN102351917A (en) * | 2011-09-14 | 2012-02-15 | 北京科技大学 | Method for extracting raffinose from cotton seed meal |
| CN102816192A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Production technology of high-purity stevioside |
| CN105153245A (en) * | 2015-09-23 | 2015-12-16 | 河南正弘药用辅料有限公司 | Production technology for medicinal cane sugar |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110656206A (en) * | 2019-09-24 | 2020-01-07 | 湖南新绿方药业有限公司 | Novel sucrose refining method capable of controlling granularity |
| CN110656206B (en) * | 2019-09-24 | 2022-11-08 | 湖南新绿方药业有限公司 | Sucrose refining method capable of controlling granularity |
| CN113956302A (en) * | 2021-11-15 | 2022-01-21 | 天津信诚康达药业有限公司 | Recrystallization method of medicinal sucrose |
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Application publication date: 20180529 |