CN103408673B - Low-ash xanthan gum and preparation method thereof - Google Patents
Low-ash xanthan gum and preparation method thereof Download PDFInfo
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- CN103408673B CN103408673B CN201310374889.5A CN201310374889A CN103408673B CN 103408673 B CN103408673 B CN 103408673B CN 201310374889 A CN201310374889 A CN 201310374889A CN 103408673 B CN103408673 B CN 103408673B
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Abstract
The invention discloses a low-ash xanthan gum and a preparation method thereof. The preparation method is used for providing a low-ash xanthan gum pharmaceutical adjuvant product by taking a food additive namely the xanthan gum as a raw material, dissolving the raw material by adopting a sorbitol aqueous solution, and refining by using ethanol. The xanthan gum prepared by the method disclosed by the invention meets pharmaceutical adjuvant requirements stated by a pharmacopoeia, and the ash content is significantly reduced at the same time, so that the low-ash xanthan gum can be widely applied to Chinese patent drugs with requirements for the ash content, the medication safety is ensured, and the application range is expanded.
Description
Technical field
The invention belongs to xanthan gum manufacturing technology field, relate to a kind of preparation method of low ash content medicinal auxiliary material xanthan gum.
Background technology
At present, xanthan gum, as joint cavity injection pharmaceutical cpd, has good viscoelasticity, good lubricating properties, and the feature such as special thixotropy of tool, can be used as excellent medicine controlled release carrier, in joint cavity, action time is lasting.Xanthan gum can also limit the position of oral pharmaceutical release, and suppresses the initial release rate of medicine, realizes colon targeting drug administration and medicament slow release.Xanthan gum has much excellent physical and chemical performance, but, investigation and application for xanthan gum pharmaceutical excipient is more late, in the control of quality product, also have a lot of drawback, and limit range of application, the ash content that such as we can see xanthan gum in 2010 editions pharmacopeia is≤16.0%, require consistent under itemizing with the ash of the first column criterion (GB13886-2007) of food-grade xanthan gum, but, for the Chinese patent medicine having ash requirements, be easy to shine into ash content and exceed standard.
Summary of the invention
The object of the invention is for medicinal auxiliary material xanthan gum ash content high, limit the problems such as the application of medicinal auxiliary material xanthan gum formulation art at home, utilize foodstuff additive xanthan gum for raw material, providing a kind of pharmaceutical excipient product by the means such as dissolving, refining.
Another object of the present invention is to provide the preparation method of this low ash content xanthan gum.
The object of the invention is to realize in the following manner:
A kind of low ash content xanthan gum, this xanthan gum prepares by the following method:
A) compound concentration is the sorbitol aqueous solution of 200 ~ 3500ppm;
B) low whipping speed is under the condition of 20 ~ 40 revs/min, in sorbitol aqueous solution, slowly add xanthan gum, and obtained concentration is 1.0 ~ 5.0%(g/ml) xanthan gum solution;
C) under agitation, in xanthan gum solution, slowly add ethanol, make solution separate out filament;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 75 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, the dry materials weightlessness obtained is 10 ~ 13%.
Preferred steps c) in, described ethanol in portions slowly add in xanthan gum solution, make filament continue separate out from solution.Be specially in step c) in, low whipping speed is under 35 ~ 50 revs/min of conditions, in xanthan gum solution, slowly add ethanol, makes the concentration of ethanol in solution 40% ~ 65%, has filament to separate out; Then adjusting stirring velocity is 10 ~ 30 revs/min, and continues slowly to add ethanol and make alcohol concn in solution be less than 85%, continues precipitation filament.Keep agitation 25 ~ 35 minutes after ethanol adds.
Xanthan gum raw material used in the present invention is food-grade xanthan gum, commercially.
The preparation method of xanthan gum solution of the present invention is under whipped state, in water, slowly add sorbyl alcohol, after sorbyl alcohol dissolves, slowly add xanthan gum, and reinforced complete continuation is stirred to xanthan gum dissolving completely.
The consumption of preferred sorbyl alcohol is 3% ~ 7% of xanthan gum quality, and the consumption of ethanol is 1.5 ~ 4.5 times of xanthan gum solution volume of water.
The preparation method of above-mentioned low ash content xanthan gum comprises the following steps:
A) compound concentration is the sorbitol aqueous solution of 200 ~ 3500ppm;
B) low whipping speed is under the condition of 20 ~ 40 revs/min, in sorbitol aqueous solution, slowly add xanthan gum, and obtained concentration is 1.0 ~ 5.0%(g/ml) xanthan gum solution;
C) under agitation, in xanthan gum solution, slowly add ethanol, make solution separate out filament;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 75 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, gained material weight loss on drying is 10 ~ 13%.
Gained xanthan gum is off-white color or buff powder; Micro-smelly, tasteless.Colloidal solution is swelled in water, insoluble in ethanol, acetone or ether.Ash content: be calculated as less than 7.5% by dry product, viscosity: the coefficient of dynamic viscosity of 25 DEG C is not less than 0.7Pa.s, pyruvic acid: the absorbancy of need testing solution is not less than the absorbancy of reference substance solution (1.6%).Nitrogen: calculate nitrogen content according to dry product and must not cross 1.4%, dry weight in wet base≤14%, heavy metal is no more than 20/1000000ths, arsenic salt≤0.0003%, microbial limit: bacterium≤800cfu/g, mould, yeast≤80cfu/g, escherichia coli, the mite that lives must not detect.
Beneficial effect of the present invention compared with the prior art:
The present invention utilizes sorbyl alcohol to promote the dissolving of xanthan gum, decreases the block in dissolution process, reduces churning time, reduces and stirs energy consumption, save production cost.Only use ethanol as Extraction medium in addition in the present invention, do not re-use the salting out that liquid caustic soda regulates pH and calcium chloride, assist the ash content reduced in product.In addition, xanthan gum of the present invention in preparation process, along with ethanol continue add, soltion viscosity reduce, adjust rotating speed in time, ensure filament fully separate out.
Significantly reduce ash oontent while the pharmaceutical excipient that the xanthan gum that the inventive method prepares meets States Pharmacopoeia specifications requires, can widespread use with for the Chinese patent medicine having ash requirements, ensure that drug safety, expand range of application.
Embodiment
The present invention is further illustrated below by way of specific embodiment.But the detail of embodiment only for explaining the present invention, should not be construed as limited overall technical solution.(Neimenggu Fufeng Biotechnologies Co., Ltd of Fu Feng group produces xanthan gum, food grade.）
Embodiment 1
A) compound concentration is the sorbitol aqueous solution of 200ppm;
B) low whipping speed is under the condition of 20 revs/min, in solution, slowly add xanthan gum, and obtained concentration is 1.%(g/ml) xanthan gum solution;
C) improving stirring velocity is 41 revs/min, slowly adds ethanol, make the concentration of ethanol in solution 40%, have filament to separate out in xanthan gum solution; Then reducing stirring velocity is 10 revs/min, and to add ethanol to alcohol concn be 50%, continues to separate out filament; After ethanol adds, the Keep agitation time is 25 minutes;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 65 DEG C ~ 75 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, material drying weight loss on drying is 10%.
The present embodiment product quality analysis: ash content: be calculated as 7.3% by dry product, the coefficient of dynamic viscosity of 25 DEG C is 1.98Pa.s, pyruvic acid: it is 4.0% that the absorbancy of need testing solution is not less than the absorbancy of reference substance solution (1.6%).Calculating nitrogen content according to dry product is 0.7%, and heavy metal is no more than 20/1000000ths, arsenic salt≤0.0003%, and microbial limit bacterium is 200cfu/g, and mould, yeast, escherichia coli, the mite that lives do not detect.
These parameters is all according to Chinese Pharmacopoeia version two ministerial standard inspection in 2010.
Embodiment 2
A) compound concentration is the sorbitol aqueous solution of 3000ppm;
B) low whipping speed is under the condition of 30 revs/min, in solution, slowly add xanthan gum, and obtained concentration is 5.0%(g/ml) xanthan gum solution;
C) improving stirring velocity is 50 revs/min, slowly adds ethanol, make the concentration of ethanol in solution 65%, have filament to separate out in xanthan gum solution; Then reducing stirring velocity is 20 revs/min, and to add ethanol to alcohol concn be 85%, continues to separate out filament; After ethanol adds, the Keep agitation time is 30 minutes;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 45 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, material drying weight loss on drying is 13%.
The present embodiment product quality analysis: ash content: be calculated as 7.45% by dry product, the coefficient of dynamic viscosity of 25 DEG C is 1.95Pa.s, pyruvic acid: it is 4.0% that the absorbancy of need testing solution is not less than the absorbancy of reference substance solution (1.6%).Calculating nitrogen content according to dry product is 0.7%, and heavy metal is no more than 20/1000000ths, arsenic salt≤0.0003%, and microbial limit bacterium is 200cfu/g, and mould, yeast, escherichia coli, the mite that lives do not detect.
These parameters is all according to Chinese Pharmacopoeia version two ministerial standard inspection in 2010.
Embodiment 3
A) compound concentration is the sorbitol aqueous solution of 1000ppm;
B) low whipping speed is under the condition of 40 revs/min, in solution, slowly add xanthan gum, and obtained concentration is 2.0%(g/ml) xanthan gum solution;
C) improving stirring velocity is 50 revs/min, slowly adds ethanol, make the concentration of ethanol in solution 50%, have filament to separate out in xanthan gum solution; Then reducing stirring velocity is 30 revs/min, and to add ethanol to alcohol concn be 75%, continues to separate out filament; After ethanol adds, the Keep agitation time is 35 minutes;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 45 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, material drying weight loss on drying is 13%.
The present embodiment product quality analysis: ash content: be calculated as 7.4% by dry product, the coefficient of dynamic viscosity of 25 DEG C is 1.99Pa.s, pyruvic acid: it is 4.0% that the absorbancy of need testing solution is not less than the absorbancy of reference substance solution (1.6%).Calculating nitrogen content according to dry product is 0.7%, and heavy metal is no more than 20/1000000ths, arsenic salt≤0.0003%, and microbial limit bacterium is 200cfu/g, and mould, yeast, escherichia coli, the mite that lives do not detect.
These parameters is all according to Chinese Pharmacopoeia version two ministerial standard inspection in 2010.
Claims (7)
1. a low-ash xanthan gum, is characterized in that this xanthan gum prepares by the following method:
A) compound concentration is the sorbitol aqueous solution of 200 ~ 3500ppm;
B) low whipping speed is under the condition of 20 ~ 40 revs/min, in sorbitol aqueous solution, slowly add xanthan gum, and obtained mass body volume concentrations g/ml is the xanthan gum solution of 1.0 ~ 5.0%;
C) under agitation, in xanthan gum solution, slowly add ethanol, make solution separate out filament;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 75 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, material drying weight loss on drying is 10 ~ 13%.
2. low-ash xanthan gum according to claim 1, is characterized in that in step c) in, described ethanol in portions slowly add in xanthan gum solution, make filament continue separate out from solution.
3. low-ash xanthan gum according to claim 1, it is characterized in that in step c) in, low whipping speed is under 35 ~ 50 revs/min of conditions, in xanthan gum solution, slowly add ethanol, make the concentration of ethanol in solution 40% ~ 65%, have filament to separate out; Then adjusting stirring velocity is 10 ~ 30 revs/min, and continues slowly to add ethanol and make alcohol concn in solution be less than 85%, continues precipitation filament.
4. low ash content xanthan gum according to claim 1, is characterized in that used xanthan gum raw material is food-grade xanthan gum.
5. low ash content xanthan gum according to claim 1, is characterized in that the consumption of described sorbyl alcohol is 3% ~ 7% of xanthan gum quality.
6. low ash content xanthan gum according to claim 1, it is characterized in that described ethanol add after Keep agitation 25 ~ 35 minutes.
7. a preparation method for low-ash xanthan gum according to claim 1, is characterized in that the method comprises the following steps:
A) compound concentration is the sorbitol aqueous solution of 200 ~ 3500ppm;
B) low whipping speed is under the condition of 20 ~ 40 revs/min, in sorbitol aqueous solution, slowly add xanthan gum, and obtained mass body volume concentrations g/ml is the xanthan gum solution of 1.0 ~ 5.0%;
C) under agitation, in xanthan gum solution, slowly add ethanol, make solution separate out filament;
D) filament of precipitation is dewatered;
E) filament after dehydration being separated is temperature 40 DEG C ~ 75 DEG C, and dry under vacuum tightness 0.02 ~ 0.10MPa condition, dry materials weightlessness is 10 ~ 13%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06157605A (en) * | 1991-04-26 | 1994-06-07 | Merck & Co Inc | Low-ash-content xanthane gum |
| CN102220393A (en) * | 2010-04-16 | 2011-10-19 | 淄博中轩生化有限公司 | Method for increasing dissolution rate of xanthan gum product |
| CN102838683B (en) * | 2012-09-18 | 2014-04-16 | 江苏神华药业有限公司 | Low molecular weight (LMW) xanthan gum and preparation method thereof |
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