CN102721783A - Method for identifying sodium salt in compound preparation - Google Patents
Method for identifying sodium salt in compound preparation Download PDFInfo
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- CN102721783A CN102721783A CN2012102166835A CN201210216683A CN102721783A CN 102721783 A CN102721783 A CN 102721783A CN 2012102166835 A CN2012102166835 A CN 2012102166835A CN 201210216683 A CN201210216683 A CN 201210216683A CN 102721783 A CN102721783 A CN 102721783A
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Abstract
The invention provides a method for identifying sodium salt in a compound preparation. The method is characterized in that besides sodium salt, the compound preparation comprises at least one or two types of calcium ions and magnesium ions. The method comprises the following steps of: excessively adding 5-20ml of 15% potassium carbonate solution into 20-50ml of sample solution; heating the mixture to a boiling point by using an electric stove; immediately putting the mixture in cold water, cooling and standing until precipitation is complete; centrifuging for 20-30 minutes at the speed of 2,500+/-100 revolutions/minute by using a centrifugal machine to obtain supernate; filtering to remove the precipitate; adding 2-6ml of potassium pyroantimonate test solution and heating the mixture to a boiling point by using the electric stove; and putting into ice water for cooling, rubbing the inner wall of a test tube with a glass rod according to requirement and determining that sodion exists if compact precipitates are generated. By the method, interference to identification of the sodium salt caused by various ions such as calcium ions and magnesium ions in the compound preparation can be avoided; moreover, the method is simple in operation; test reagents and utensils are readily available, and test results are obvious.
Description
Technical field
The present invention relates to the drug inspection technical field, is the discrimination method of sodium salt in a kind of compound preparation, mainly is in need testing solution, to contain different kinds of ions such as magnesium, calcium simultaneously sodium salt is differentiated that the method for inspection of using when disturbing is arranged.
Background technology
Existing a kind of novel compound preparation, its solvent is a water, contains sodium chloride, potassium chloride, lime chloride, magnesium chloride, sodium acetate and sodium citrate in the prescription.According to national relevant regulations, should comprise the wherein discrimination test of various ion components in the quality standard of this compound preparation, but make an experiment according to two kinds of methods of sodium salt identification in two appendix III of the version Pharmacopoeia of the People's Republic of China in 2010:
(1) get platinum filament, with hydrochloric acid wetting after, dip in and get test sample, in colourless flame, burn, flame promptly shows foresythia.
(2) get the about 100mg of test sample, put in the 10ml test tube, add water 2ml dissolving, add 15% solution of potassium carbonate 2ml, be heated to and boil, should have deposition to generate; Add potassium pyroantimonate test solution 4ml, be heated to and boil; To frozen water, cool off, in case of necessity,, should have fine and close deposition to generate with the glass rod inboard wall of test tube that rubs.
Its test findings is distinguished as follows:
1. discrimination test (1): the foresythia phenomenon is not obvious.
2. discrimination test (2): get the about 100mg of test sample, put in the 10ml test tube, add water 2ml dissolving, add 15% solution of potassium carbonate 2ml, be heated to and boil, have a large amount of white flocculent deposits to generate, test can't be proceeded.
Analyzing reason mainly is:
1. in the discrimination test (1), potassium chloride, lime chloride have interference to the discriminating of sodium salt.According to the test method in the version Pharmacopoeia of the People's Republic of China in 2010 two appendix III: the identification of calcium salt, get platinum filament, with hydrochloric acid wetting after, dip in and get test sample, in colourless flame, burn, flame is promptly apparent brick-red; Platinum filament is got in the identification of sylvite, with hydrochloric acid wetting after, dip in and get test sample, in colourless flame, burn, flame promptly shows purple, but has a spot of sodium salt to mix when depositing, and must can recognize at a distance from the blue tinted glass perspective.Therefore, when having sodium, potassium, calcium ion simultaneously in the need testing solution, the foresythia of sodium itself is just difficult to be differentiated, and makes experimental phenomena not obvious.
2. precipitate owing to lime chloride, magnesium chloride all can produce with sal tartari in the discrimination test (2), test can't be carried out, the existence of mentioned component has produced interference to the discriminating of sodium salt.
Above test findings proves; The method that sodium salt is differentiated in two appendix III of the version Pharmacopoeia of the People's Republic of China in 2010 is only applicable to the sodium salt of one matter and differentiates; Be not suitable for novel compound preparation; And the discrimination method of sodium salt is not reported in this type of compound preparation, therefore, lacks a kind of effective, easy and simple to handle method to sodium salt in the compound preparation is differentiated at present.
Summary of the invention
The present invention is for solving the problem that prior art exists; The discrimination method of sodium salt in a kind of compound preparation is provided, can avoids calcium, magnesium plasma in the compound preparation that sodium salt is differentiated that interference is arranged, simple to operate; Test reagent and apparatus are common to be easy to get, and experimental phenomena is obvious.
The objective of the invention is to realize: the discrimination method of sodium salt in a kind of compound preparation through following technical scheme; It is characterized in that; Said compound preparation and contains one or both ions in calcium ion, the magnesium ion at least except that containing sodium salt, discrimination method may further comprise the steps:
(1) get need testing solution 20-50ml, excessive adding 15% solution of potassium carbonate 5-20ml, electric furnace is heated to and boils; Cooling is left standstill and is made deposition fully to the frozen water at once; With hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, remove by filter sediment;
(2) add potassium pyroantimonate test solution 2-6ml, electric furnace is heated to and boils;
(3) to frozen water, cool off, have fine and close deposition to generate, prove that sodion exists.
Improvement to technique scheme: in the said step (3), cooling is at least 30 minutes to the frozen water, with the glass rod inboard wall of test tube that rubs.
Further improvement to technique scheme:
Every 1000ml prescription of said compound preparation is:
Concrete discrimination method is:
Get need testing solution 35ml, excessive adding 15% solution of potassium carbonate 10ml, electric furnace is heated to and boils, cooling is left standstill and is made deposition fully to the frozen water at once, with hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, remove by filter sediment; Add potassium pyroantimonate test solution 4ml, electric furnace is heated to and boils; To frozen water, cool off, in case of necessity,, should have fine and close deposition to generate, prove the sodion existence with the glass rod inboard wall of test tube that rubs.
The present invention compared with prior art has following advantage and good effect:
Discrimination method of the present invention can avoid different kinds of ions such as the calcium, magnesium in the compound preparation that sodium salt is differentiated that interference is arranged, and simple to operate, test reagent and apparatus are common to be easy to get, and experimental phenomena is obvious.
To the checking that makes an experiment of the multiple sodium salt compound preparation that contains materials such as lime chloride, magnesium chloride simultaneously, the method all is suitable for as a result according to this method.Show that thus this method is applicable to the identification of sodium salt in the polycomponent compound preparations such as containing calcium ion, magnesium ion simultaneously.
Embodiment
The embodiment of the discrimination method of sodium salt in a kind of compound preparation of the present invention, said compound preparation and contain one or both ions in calcium ion, the magnesium ion at least except that containing sodium salt, discrimination method may further comprise the steps:
(1) get need testing solution 20-50ml, excessive adding 15% solution of potassium carbonate 5-20ml, electric furnace is heated to and boils; Cooling is left standstill and is made deposition fully to the frozen water at once; With hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, remove by filter sediment;
(2) add potassium pyroantimonate test solution 2-6ml, electric furnace is heated to and boils;
(3) to frozen water, cool off, have fine and close deposition to generate, prove that sodion exists.
In step (3), to the frozen water in the cooling procedure, in case of necessity, with the glass rod inboard wall of test tube that rubs.
The discrimination method of sodium salt specific embodiment in the compound preparation of the present invention:
Every 1000ml of compound preparation writes out a prescription as follows:
Process of the test is following:
1. get test sample 35ml in small beaker, excessive adding 15% solution of potassium carbonate 10ml, electric furnace is heated to and boils, and cooling makes deposition fully to the frozen water at once.
With hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, filter paper filtering adds potassium pyroantimonate test solution 4ml, electric furnace is heated to and boils; Cooling (half an hour at least) to the frozen water, deposition more after a little while, with the glass rod inboard wall of test tube that rubs, viewing test phenomenon.There is fine and close deposition to generate, proves that sodion exists.
The preparation negative sample contrasts synchronously, and test findings is following:
Above-mentioned test findings shows, truly has sodion to exist in the test sample.This test method is effective, and is easy and simple to handle, and this method through the Shandong Province food and medicine check be expounded through peer review through.
Certainly, above-mentioned explanation is not to be the restriction to invention, and the present invention also is not limited to above-mentioned giving an example, those skilled in the art, and the variation of in essential scope of the present invention, making, remodeling, interpolation or replacement also should belong to protection scope of the present invention.
Claims (3)
1. the discrimination method of sodium salt in the compound preparation is characterized in that, said compound preparation and contains one or both ions in calcium ion, the magnesium ion at least except that containing sodium salt, and discrimination method may further comprise the steps:
(1) get need testing solution 20-50 ml, excessive adding 15% solution of potassium carbonate 5-20 ml, electric furnace is heated to and boils; Cooling is left standstill and is made deposition fully to the frozen water at once; With hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, remove by filter sediment;
(2) add potassium pyroantimonate test solution 2-6ml, electric furnace is heated to and boils;
(3) to frozen water, cool off, have fine and close deposition to generate, prove that sodion exists.
2. according to the discrimination method of sodium salt in the described compound preparation of claim 1, it is characterized in that in the said step (3), cooling is at least 30 minutes to the frozen water, with the glass rod inboard wall of test tube that rubs.
3. according to the discrimination method of sodium salt in claim 1 or the 2 described compound preparations, it is characterized in that concrete steps are following:
Per 1000 ml prescription of said compound preparation is:
Sodium chloride 6.40g
Potassium chloride 0.75g
Lime chloride 0.48g
Magnesium chloride 0.30g
Sodium acetate 3.90g
Sodium citrate 1.70g
Water for injection is an amount of
Concrete discrimination method is:
Get need testing solution 35 ml, excessive adding 15% solution of potassium carbonate 10 ml, electric furnace is heated to and boils, cooling is left standstill and is made deposition fully to the frozen water at once, with hydro-extractor with the centrifugal 20～30min of 2500 ± 100r/min after, get supernatant, remove by filter sediment; Add potassium pyroantimonate test solution 4ml, electric furnace is heated to and boils; To frozen water, cool off,, have fine and close deposition to generate, prove the sodion existence with the glass rod inboard wall of test tube that rubs.
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| CN2012102166835A CN102721783A (en) | 2012-06-27 | 2012-06-27 | Method for identifying sodium salt in compound preparation |
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| CN2012102166835A CN102721783A (en) | 2012-06-27 | 2012-06-27 | Method for identifying sodium salt in compound preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588835A (en) * | 2014-10-23 | 2016-05-18 | 华仁药业股份有限公司 | A method of identifying a magnesium salt in a compound preparation containing gluconic acid radicals |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1775811A (en) * | 2005-11-30 | 2006-05-24 | 史美丽 | Taro starch extracting method |
| CN101161812A (en) * | 2006-10-13 | 2008-04-16 | 上海中港亚诺化学技术有限公司 | Streptococcus separating method for kabikinase fermentation liquor |
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- 2012-06-27 CN CN2012102166835A patent/CN102721783A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1775811A (en) * | 2005-11-30 | 2006-05-24 | 史美丽 | Taro starch extracting method |
| CN101161812A (en) * | 2006-10-13 | 2008-04-16 | 上海中港亚诺化学技术有限公司 | Streptococcus separating method for kabikinase fermentation liquor |
Non-Patent Citations (2)
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| QINGMEI7: "钠盐鉴别实验", 《百度文库》 * |
| 国家药典委员会: "《中华人民共和国药典：2010年版.二部》", 31 January 2010, 中国医药科技出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588835A (en) * | 2014-10-23 | 2016-05-18 | 华仁药业股份有限公司 | A method of identifying a magnesium salt in a compound preparation containing gluconic acid radicals |
| CN105588835B (en) * | 2014-10-23 | 2019-01-04 | 华仁药业股份有限公司 | The discrimination method of magnesium salts in the compound preparation of the acid group containing glucose |
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Application publication date: 20121010 |