CN102221596A - Method for quickly detecting reality and purity of glucosamine sulfate and potassium chloride - Google Patents
Method for quickly detecting reality and purity of glucosamine sulfate and potassium chloride Download PDFInfo
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- CN102221596A CN102221596A CN2011100912009A CN201110091200A CN102221596A CN 102221596 A CN102221596 A CN 102221596A CN 2011100912009 A CN2011100912009 A CN 2011100912009A CN 201110091200 A CN201110091200 A CN 201110091200A CN 102221596 A CN102221596 A CN 102221596A
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Abstract
The invention relates to a method for quickly detecting reality and purity of glucosamine sulfate and potassium chloride, comprising the following steps: obtaining an organic solvent with the specific weight of 2.0 to 2.6 or more than two organic solvents to prepare 10ml of organic solution with the specific weight of 2.0 to 2.6; adding 2g of glucosamine sulfate and potassium chloride complying with American FDA standard; acutely shaking the solution; and keeping the solution standing for 10 minutes at the room temperature and observing the solution. If white powder floats on the surface of the organic solvent and deposits do not exist at the bottom of the organic solvent, the sample is proved to be the glucosamine sulfate and potassium chloride; and if the white powder does not float on the surface of the solution and a large amount of deposits exist at the bottom of the solution, the sample is proved not to be the glucosamine sulfate and potassium chloride, but the mixture of glucosamine hydrochloride and the potassium chloride, and the deposits are potassium sulfate. If trace depositions or no deposits exist at the bottom of the solution and flocculant exists in the solution, the product is proved to have low purity. The method can detect the reality and the purity of glucosamine sulfate and potassium chloride simply and visually.
Description
Technical field
The present invention relates to the detection of Glucosamine Sulphate potash chlorate, the method for particularly a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity
Background technology
Glucosamine Sulphate potassium chloride (Glucosamine Potassium Sulfate), molecular formula: (C
6H
14NO
5)
2SO
4.2KCl, molecular weight: 605.52.
Glucosamine Sulphate potassium chloride is the osteoarthrosis nutritious supplementary pharmaceutical of generally acknowledging in the world at present, and medicine of treatment osteoarthrosis in is listed it by nearly 40 countries.U.S. FDA was listed pharmacopeia in 1997 in, and European Union listed pharmacopeia in 1999 in.At present, understand, have two kinds of production technologies to produce and meet the product of (U.S. FDA etc.) and China " Glucosamine Sulphate potassium chloride " bulk drug standard abroad according to us.A kind of is ion exchange process, and another kind is the physics method of double crossing.The manufacturing process of ion exchange process is to be raw material with aminoglucose hydrochloride and sulfuric acid, potassium chloride or glazier's salt, under given conditions, pass through ion exchange technique, aminoglucose hydrochloride is changed into Glucosamine Sulphate, make Glucosamine Sulphate and potassium chloride form stable eutectic thing at last, this is a kind of technology that higher technical difficulty is arranged.The physics method of double crossing is exactly with sieving after aminoglucose hydrochloride and the glazier's salt pulverizing, and is composite in the ratio of 2.5:1 then, and material is fully mixed.The product of these two kinds of method preparations detects every can both meeting the requirements according to relevant " Glucosamine Sulphate potassium chloride technical indicator " in the present world standard, yet its essence is the product of two completely different (drug effects).Glucosamine Sulphate potassium chloride drug effect significantly and the curative effect of aminoglucose hydrochloride is general.Because the Glucosamine Sulphate pharmacological action realizes jointly by Glucosamine and sulfate ion.No matter inject or oral Glucosamine Sulphate after, can find in the serum that the sulfate radical level increases, and the sulfate ion in the serum is being controlled the synthesis rate of gucosamine and proteoglycans, wherein proteoglycans becomes the part of cartilage matrix.Sulfate radical is also for the utilization of aminoglucose resource provides support in the building-up process of cartilage, and owing to the existence of sulfate radical in the serum has increased this product anti-inflammatory and analgesic effect.And aminoglucose hydrochloride is compared pharmacologically active with Glucosamine Sulphate much lower, and glazier's salt composition wherein is exactly a mineral sulfates in fact, wherein the inorganic sulfur acid group originally can not enter in the blood of human body and act synergistically with the Glucosamine performance, the main cause of both the drug effect difference that our front clinical trial that Here it is is verified, and wherein glazier's salt is owing to be chemical reagent, and long-term a large amount of edible harm that human liver, kidney are caused are conspicuous.
" Glucosamine Sulphate potassium chloride " market demand is very big, and every year, nearly in the world several hundred million people took this product, and global annual turnover is more than 30,000 tons.Existing a lot of manufacturing enterprises all are according to U.S. FDA standard manufacture " Glucosamine Sulphate potassium chloride " product, so a lot of technical indicator conformance with standard can occur on the market, but reality is not the product of Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt.This is the wine of 52 degree just as making wine equally, and a kind of is to blend with alcohol and water, a kind of brewageing, and this is also the same with mixing melamine in the milk powder, and one is to replace protein with melamine, and one is used glazier's salt to replace Glucosamine Sulphate.Controlled its true and false and purity so be starved of and set up a complete detection method, for human health is benefited.
Summary of the invention
Goal of the invention
The present invention is a method of having set up a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity.This method is from comparing the proportion of the composite Glucosamine Sulphate potassium chloride of Glucosamine Sulphate potassium chloride double salt and physics, observation sample in organic solvent state and set up a kind of method for quick, thereby really control the quality and stability, the medicine of the Glucosamine Sulphate potassium chloride of stopping to palm off of Glucosamine Sulphate crystalline drug.
Technical scheme
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be 2.0~2.6 organic solvent 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt;
B, to get proportion be 2.0 organic solvent 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
Described organic solvent is methylene bromide, methylene chloride, methenyl choloride any one or two or more potpourri arbitrarily.
As the described organic solvent of a kind of optimal way is methenyl choloride and methylene chloride mixed solvent, methylene bromide and methylene chloride mixed solvent or methylene bromide and methenyl choloride mixed solvent.
Beneficial effect
1, this patent method analysis: utilize the organic solvent deposit detection method: can detect at first that " Glucosamine Sulphate potassium chloride sample is the Glucosamine Sulphate potassium chloride crystallization for preparing after the ion-exchange or mixes the sample for preparing by aminoglucose hydrochloride and glazier's salt.Detect by organic solvent, we can also observe the purity of Glucosamine Sulphate potassium chloride, because we discover that the density of Glucosamine Sulphate potassium chloride is 0.92g/cc, the density of glazier's salt is 2.662g/cc, the density of potassium chloride is 1.96g/cc, the density of salt acidic group glucose is 0.62g/cc, organic solvent in preparation 2.0 g/cc density experimentizes, real Glucosamine Sulphate potassium chloride crystallization all swims in the upper strata of solvent, and the potpourri that makes by physical method, aminoglucose hydrochloride all swims in the upper strata of solvent, and glazier's salt then all is deposited in the bottom of organic solvent.Can obtain the Glucosamine Sulphate potassium chloride true and false by the simple, intuitive observation detects.
, present international Glucosamine Sulphate potassium chloride technical standard all is to work out with reference to the standard of U.S. FDA basically, the key technical indexes has following four aspects:
1) content 98 ~ 102%, and 2) optical activity :+50 ° ~ 52 °, 3) ignition residue 27 ~ 29%, 4) pH value: 3.5 ~ 4.5.The standard that the U.S. works out, is exactly a qualified product, otherwise is exactly substandard product as long as the technical indicator of this product meets above standard according to this product face speech of Glucosamine Sulphate potassium chloride.But U.S. FDA is not considered be aminoglucose hydrochloride and glazier's salt in the composite potpourri of the ratio of 2.5:1, equally also meet 4 technical indicators of Glucosamine Sulphate potassium chloride.
We can detect the content from four and find out why at present standard is difficult to differentiate true and false Glucosamine Sulphate potassium chloride.
1), content: 98 ~ 102%, if content detection is a tester by aminoglucose hydrochloride, that chlorion is to represent weight indicator of content, the true product of no matter ion-exchange manufactured, still all contain chlorion with the composite false pain product of 2.5:1 ratio with standard, generally 11 ~ 13%, being calculated to be content is 98 ~ 102%.
2), optical activity: the optical activity of qualified Glucosamine Sulphate potassium chloride is+50
o~ 52
oAnd in the composite false pain product of 2.5:1 ratio, optical activity also is+50
o~ 52
oBecause the optical activity of pure hydrochloric acid Glucosamine is+71 ~ 73, and aminoglucose hydrochloride accounts for 72% in the potpourri of 2.5:1, in fact potpourri+50
o~ 52
oOptical activity is exactly the optical activity that accounts for 72% aminoglucose hydrochloride, so both are easy to obscure.
3), ignition residue: the ignition residue of the Glucosamine Sulphate potassium chloride in the standard is 27 ~ 29%, and its essence of this residue is exactly the content of sulfate radical and potassium.The content of glazier's salt is 28% in the potpourri of 2.5:1, so potpourri reaches this index very like a cork.
4), pH value: 3.5 ~ 4.5, no matter be qualified Glucosamine Sulphate potassium chloride or composite aminoglucose hydrochloride glazier's salt, its hydrogen ion content is the same, so pH value also is identical.
We think that the standard that U.S. FDA, European Union set up is at this product, meet 4 technical indicators stipulating in the existing standard as long as that is to say Glucosamine Sulphate ammonification potassium, are exactly specification product.But, there are a lot of producers to manufacture a product at present according to the U.S. FDA standard, so on market, a lot of technical indicator conformance with standard can occur, but reality is not the product of Glucosamine Sulphate potassium chloride, but potpourri of aminoglucose hydrochloride and glazier's salt.
For standard Glucosamine Sulphate potassium chloride market, health for whole mankind's osteoarthrosis people, stop counterfeit and shoddy goods, the technical standard of Glucosamine Sulphate potassium chloride is improved and improved in our ad hoc proposal relevant department, and rise to international standard, make our contribution for the human beings'health cause.
Embodiment
Glucosamine Sulphate potassium chloride double salt (a) is two vast stretches of wooded country ocean, Jiangsu Bioceuticals Inc. product, and the composite Glucosamine Sulphate potassium chloride (b) of physics is that aminoglucose hydrochloride adds glazier's salt and gets in the composite preparation of the ratio of 2.5:1.
Embodiment 1
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be that proportion that 2.0~2.6 organic solvent or two or more organic solvent are mixed with is 2.0 ~ 2.6 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt.
B, to get proportion be that proportion that 2.0 organic solvent or two or more organic solvent are mixed with is 2.0 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
Wherein organic solvent is a methenyl choloride.
Embodiment 2
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be that proportion that 2.0~2.6 organic solvent or two or more organic solvent are mixed with is 2.0 ~ 2.6 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt.
B, to get proportion be that proportion that 2.0 organic solvent or two or more organic solvent are mixed with is 2.0 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
The further preferred embodiment organic solvent is a methylene bromide.
Embodiment 3
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be that proportion that 2.0~2.6 organic solvent or two or more organic solvent are mixed with is 2.0 ~ 2.6 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt.
B, to get proportion be that proportion that 2.0 organic solvent or two or more organic solvent are mixed with is 2.0 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
Wherein organic solvent is a methylene chloride.
Embodiment 4
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be that proportion that 2.0~2.6 organic solvent or two or more organic solvent are mixed with is 2.0 ~ 2.6 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt.
B, to get proportion be that proportion that 2.0 organic solvent or two or more organic solvent are mixed with is 2.0 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
Wherein organic solvent is methenyl choloride and methylene chloride mixed solvent.
Embodiment 5
The method of a kind of fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that
A, to get proportion be that proportion that 2.0~2.6 organic solvent or two or more organic solvent are mixed with is 2.0 ~ 2.6 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt.
B, to get proportion be that proportion that 2.0 organic solvent or two or more organic solvent are mixed with is 2.0 organic solution 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
Wherein organic solvent is methylene bromide and methylene chloride mixed solvent.
Checking example 6
The Glucosamine Sulphate potassium chloride sample that meets the U.S. FDA standard among the foregoing description 1-5 is that Glucosamine Sulphate potassium chloride double salt (a) and aminoglucose hydrochloride add the composite Glucosamine Sulphate potassium chloride (b) of glazier's salt physics, and both all meet the FDA standard promptly for it:
1), content: 98 ~ 102%;
2), optical activity: the optical activity of qualified Glucosamine Sulphate potassium chloride is+50 ~ 52;
3), ignition residue content: the ignition residue of the Glucosamine Sulphate potassium chloride in the standard is 27 ~ 29%;
4), pH value: 3.5 ~ 4.5;
But both x monocrystalline derivative data differences, confirm two kinds of material differences from structural level: the Glucosamine Sulphate potassium chloride of preparation (ion-exchange obtains Glucosamine Sulphate potassium chloride double salt a and the composite acquisition Glucosamine Sulphate of physics potassium chloride b) detects through the X diffraction, and its result is:
? | GSPC* | GSPC* |
Peak | a | b |
100% | 7.063 | 5.112 |
2nd?Peak | 2.887 | 3.282 |
3rd? Peak | 3.510 | 7.098 |
4th? Peak | 3.549 | 3.562 |
5th? Peak | 2.603 | 5.331 |
* GSPC=Glucosamine Sulfate Potassium Chloride(Glucosamine Sulphate potassium chloride)
Claims (3)
1. the method for the fast detecting Glucosamine Sulphate potassium chloride true and false and purity is characterized in that:
A, to get proportion be 2.0~2.6 organic solvent 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder of organic solvent is floating, the bottom does not have sediment, proves that then this sample is a Glucosamine Sulphate potassium chloride; If the surperficial adularescent powder of solution is floating, a large amount of sediments is arranged at the bottom, proves that then this sample is not a Glucosamine Sulphate potassium chloride, but the potpourri of aminoglucose hydrochloride and glazier's salt, sediment is a glazier's salt;
B, to get proportion be 2.0 organic solvent 10ml, add Glucosamine Sulphate potassium chloride sample 2 grams that meet the U.S. FDA standard, concuss, room temperature left standstill after 10 minutes observes, if the surperficial adularescent powder in the solution is floating, the microprecipitation thing is arranged at the bottom, or the bottom does not have sediment, but a spot of flocculation material is arranged in the solution, prove that then Glucosamine Sulphate potassium chloride purity is not high in the sample.
2. the method for a kind of fast detecting Glucosamine Sulphate potassium chloride true and false according to claim 1 and purity is characterized in that described organic solvent is methylene bromide, methylene chloride, methenyl choloride any one or two or more potpourri arbitrarily.
3. the method for a kind of fast detecting Glucosamine Sulphate potassium chloride true and false according to claim 2 and purity is characterized in that described organic solvent is methenyl choloride and methylene chloride mixed solvent, methylene bromide and methylene chloride mixed solvent or methylene bromide and methenyl choloride mixed solvent.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102866235A (en) * | 2012-10-15 | 2013-01-09 | 江苏澳新生物工程有限公司 | Detection method for D-glucosamine sulfate |
CN112461707A (en) * | 2020-11-28 | 2021-03-09 | 江苏盐城津能电力有限公司 | Inspection formula solution for plastic cable protection pipe |
Citations (4)
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US5843923A (en) * | 1998-05-22 | 1998-12-01 | Jame Fine Chemicals, Inc. | Glucosamine sulfate potassium chloride and process of preparation thereof |
US5902801A (en) * | 1998-05-22 | 1999-05-11 | Jame Fine Chemicals, Inc. | Glucosamine sulfate metal chloride compositions and process of preparing same |
CN1736613A (en) * | 2005-06-17 | 2006-02-22 | 东南大学 | Deposition-floatation method for separating solid multi-phase mixture |
CN101012251A (en) * | 2007-01-11 | 2007-08-08 | 庄建华 | Method of preparing aminoglucose composite sulphate |
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2011
- 2011-04-13 CN CN2011100912009A patent/CN102221596A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US5843923A (en) * | 1998-05-22 | 1998-12-01 | Jame Fine Chemicals, Inc. | Glucosamine sulfate potassium chloride and process of preparation thereof |
US5902801A (en) * | 1998-05-22 | 1999-05-11 | Jame Fine Chemicals, Inc. | Glucosamine sulfate metal chloride compositions and process of preparing same |
CN1736613A (en) * | 2005-06-17 | 2006-02-22 | 东南大学 | Deposition-floatation method for separating solid multi-phase mixture |
CN101012251A (en) * | 2007-01-11 | 2007-08-08 | 庄建华 | Method of preparing aminoglucose composite sulphate |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102866235A (en) * | 2012-10-15 | 2013-01-09 | 江苏澳新生物工程有限公司 | Detection method for D-glucosamine sulfate |
CN102866235B (en) * | 2012-10-15 | 2014-12-24 | 江苏澳新生物工程有限公司 | Detection method for D-glucosamine sulfate |
CN112461707A (en) * | 2020-11-28 | 2021-03-09 | 江苏盐城津能电力有限公司 | Inspection formula solution for plastic cable protection pipe |
CN112461707B (en) * | 2020-11-28 | 2023-01-17 | 江苏盐城津能电力有限公司 | Inspection formula solution for plastic cable protection pipe |
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Application publication date: 20111019 |