CN102507568A - Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt - Google Patents
Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt Download PDFInfo
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- CN102507568A CN102507568A CN2011103000442A CN201110300044A CN102507568A CN 102507568 A CN102507568 A CN 102507568A CN 2011103000442 A CN2011103000442 A CN 2011103000442A CN 201110300044 A CN201110300044 A CN 201110300044A CN 102507568 A CN102507568 A CN 102507568A
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- sodium thiosulfate
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Abstract
The invention relates to a method for detecting the content of cis-propenyl phophonic acid in a phosphate-ammonium salt, belonging to the field of medicament analysis. The method comprises the following steps: preparing iodine chloride reagent: dissolving 8g of iodine trichloride in 200ml of glacial acetic acid, dissolving 9g of iodine in 300ml of glacial acetic acid, mixing two solutions, adding glacial acetic acid to dilute the mixed solution to the volume of 1,000ml and shaking uniformly; preparing starch indicating solution; weighting 0.5g of soluble starch, adding 5ml of water, stirring uniformly, pouring the mixture into 100ml of boiling water, continuing to boil for 2min, standing to cool, and taking supernatant; and preparing 0.1mol/L sodium thiosulfate titrant: weighting 26g of sodium thiosulfate and 0.20g of anhydrous sodium carbonate, adding a proper amount of cooled boiled water to dissolve and dilute to the volume of 1,000ml, shaking uniformly, standing, and filtering. The method adopts the chemical titration process, has the advantages of rapidness, accuracy and low cost and is suitable for real-time control of the mass of the intermediates in the production process.
Description
Technical field
The present invention relates to cis-propene phosphoric acid content detecting method in a kind of fosfomycin phenylethylamine calt in the Pharmaceutical Analysis field.
Background technology
Fosfomycin sodium [(-)-suitable-1; 2-phosphate epoxypropyl sodium] be a kind of New-type wide-spectrum antibiotic; Its bactericidal action mechanism is suppress bacteria cell wall early stage synthetic, with pharmaceutical research proof fosfomycin sodium most of gram-positive bacterias and Gram-negative bacteria is had stronger bactericidal action through clinical, and can get in the cerebrospinal fluid through blood-brain barrier; Have no antigen, little, the good chemical stability of toxicity, be applicable to internal medicine, paediatrics, ENT dept., urological department etc.1R2s-(-)-suitable-1,2-phosphate epoxypropyl-R-(+)-α-Ben Yian salt, promptly fosfomycin phenylethylamine calt is a kind of important intermedium in the chemosynthesis fosfomycin sodium process, its impurity content directly influences the quality of downstream product.If the intermedium cis-propene phosphoric acid too high levels in residual preceding step is with the quality that has a strong impact on fosfomycin phenylethylamine calt, particularly remarkable with bad stability in the fosfomycin phenylethylamine calt.For guaranteeing the quality and the security thereof of medicine, need set up detection method the content of cis-propene phosphoric acid in the fosfomycin phenylethylamine calt is controlled.At present, about to cis-propene phosphoric acid content detecting method in the fosfomycin phenylethylamine calt, do not see relevant report.Therefore, develop that the cis-propene phosphoric acid content detecting method is the new problem that needs to be resolved hurrily always in a kind of fosfomycin phenylethylamine calt.
Summary of the invention
The object of the present invention is to provide cis-propene phosphoric acid content detecting method in a kind of fosfomycin phenylethylamine calt, this method adopts chemical titration, is characterized in that fast, accurately, expense is low, is applicable to the real-time control of production run intermedium quality.
The objective of the invention is to realize like this: cis-propene phosphoric acid content detecting method in a kind of fosfomycin phenylethylamine calt, this detection method comprises the steps:
(1) preparation of iodine monochloride reagent: dissolving 8g iodine trichloride is in the 200ml glacial acetic acid, and dissolving 9g iodine mixes above-mentioned two kinds of solution in the 300ml glacial acetic acid, adds glacial acetic acid and is diluted to 1000ml, shakes up;
(2) preparation of starch indicator solution: get soluble starch 0.5g, after adding water 5ml and stirring, in the impouring 100ml boiling water, continued to boil 2 minutes, put coldly, get supernatant liquor;
(3) preparation of 0.1mol/L sodium thiosulfate vs: get sodium thiosulfate 26g and natrium carbonicum calcinatum 0.20g, add the cold water that newly boiled and make dissolving in right amount and be diluted to 1000ml, shake up, place the back and filter;
(4) demarcation of sodium thiosulfate vs: be taken at 120 ℃ of base weight potassium chromate 0.15g that are dried to constant weight, put in the iodine flask, add water 50ml and make dissolving, add potassium iodide 2.0g, add dilute sulfuric acid 40ml after the dissolving, shake up close plug; After in the dark placing 10 minutes, add water 250ml dilution, during with sodium thiosulfate vs titration near terminal point; Add starch indicator solution 3ml; Continue titration to blue the disappearance and show bright green, and the result of titration is proofreaied and correct with blank test, every 1ml sodium thiosulfate vs is equivalent to the potassium dichromate of 4.903mg; According to the amount of taking of the consumption and the potassium dichromate of sodium thiosulfate vs, the concentration that calculates the sodium thiosulfate vs is C mol/L;
(5) take by weighing confession test agent 2.0g; Place iodine flask, add the 20ml glacial acetic acid, add 15ml iodine monochloride reagent again; Shake up; In the dark place after 60 minutes and to add 20ml 50% potassium iodide reagents, when light yellow, the volume that writes down consume sulfur sodium thiosulfate vs is V with the titration of 0.1mol/L sodium thiosulfate vs
1Ml adds 2ml starch indicator solution, continues titration and disappears to blue, does blank test simultaneously, and the volume of record consume sulfur sodium thiosulfate vs is V
0Ml;
(6) supply the computing formula of cis-propene phosphoric acid content in the test agent to be:
V
0: the volume of blank consume sulfur sodium thiosulfate vs, ml;
V
1: sample solution consumes the volume of consume sulfur sodium thiosulfate vs, ml;
C: the concentration of sodium thiosulfate vs, mol/L;
W: the weight of test sample, mg.
Main points of the present invention are its detection method.Its principle of work is; To supply to add in the test agent glacial acetic acid, iodine monochloride reagent, potassium iodide reagents; With the titration of sodium thiosulfate vs when light yellow; Add the starch indicator solution, continue titration and disappear, mainly adopt chemical titration to measure the content of cis-propene phosphoric acid in the fosfomycin phenylethylamine calt to blue.
In a kind of fosfomycin phenylethylamine calt the cis-propene phosphoric acid content detecting method compared with prior art, this method adopts chemical titration, is characterized in quick; Accurately; Expense is low, is applicable to the advantages such as real-time control of production run intermedium quality, will be widely used in the Pharmaceutical Analysis field.
Embodiment
Following instance will help understanding of the present invention, but these instances have been merely and the present invention are explained the present invention is not limited to these contents.
(1) preparation of iodine monochloride reagent: dissolving 8g iodine trichloride is in the 200ml glacial acetic acid, and dissolving 9g iodine mixes above-mentioned two kinds of solution in the 300ml glacial acetic acid, adds glacial acetic acid and is diluted to 1000ml, shakes up;
(2) preparation of starch indicator solution: get soluble starch 0.5g, after adding water 5ml and stirring, in the impouring 100ml boiling water, continued to boil 2 minutes, put coldly, get supernatant liquor;
(3) preparation of 0.1mol/L sodium thiosulfate vs: get sodium thiosulfate 26g and natrium carbonicum calcinatum 0.20g, add the cold water that newly boiled and make dissolving in right amount and be diluted to 1000ml, shake up, place the back and filter;
(4) demarcation of sodium thiosulfate vs: be taken at 120 ℃ of base weight potassium chromate 0.15g that are dried to constant weight, put in the iodine flask, add water 50ml and make dissolving, add potassium iodide 2.0g, add dilute sulfuric acid 40ml after the dissolving, shake up close plug; After in the dark placing 10 minutes, add water 250ml dilution, during with sodium thiosulfate vs titration near terminal point; Add starch indicator solution 3ml; Continue titration to blue the disappearance and show bright green, and the result of titration is proofreaied and correct with blank test, every 1ml sodium thiosulfate vs is equivalent to the potassium dichromate of 4.903mg; According to the amount of taking of the consumption and the potassium dichromate of sodium thiosulfate vs, the concentration that calculates the sodium thiosulfate vs is C mol/L.
Embodiment 1
Take by weighing and supply test agent 2.0008g, place the 250ml iodine flask, add the 20ml glacial acetic acid, the accurate again 15ml iodine monochloride reagent that adds closes the lid, and shakes up.In the dark placed 60 minutes.Add 20ml 50% potassium iodide reagents; With sodium thiosulfate vs (0.09668mol/L) titration when light yellow; Add 2ml starch indicator solution, continue titration and disappear to blue, recording volume is 27.30ml (proofreading and correct the back); Do blank test simultaneously, the volume of record consume sulfur sodium thiosulfate vs is 28.82ml (proofreading and correct the back).
Supply the computing formula of cis-propene phosphoric acid content in the test agent to be:
Embodiment 2
Take by weighing and supply test agent 2.0031g, place the 250ml iodine flask, add the 20ml glacial acetic acid, the accurate again 15ml iodine monochloride reagent that adds closes the lid, and shakes up.In the dark placed 60 minutes.Add 20ml 50% potassium iodide reagents; With sodium thiosulfate vs (0.09668mol/L) titration when light yellow; Add 2ml starch indicator solution, continue titration and disappear to blue, recording volume is 27.12ml (proofreading and correct the back); Do blank test simultaneously, the volume of record consume sulfur sodium thiosulfate vs is 28.82ml (proofreading and correct the back).
Supply the computing formula of cis-propene phosphoric acid content in the test agent to be:
Embodiment 3
Take by weighing and supply test agent 2.0027g, place the 250ml iodine flask, add the 20ml glacial acetic acid, the accurate again 15ml iodine monochloride reagent that adds closes the lid, and shakes up.In the dark placed 60 minutes.Add 20ml 50% potassium iodide reagents; With sodium thiosulfate vs (0.09668mol/L) titration when light yellow; Add 2ml starch indicator solution, continue titration and disappear to blue, recording volume is 27.72ml (proofreading and correct the back); Do blank test simultaneously, the volume of record consume sulfur sodium thiosulfate vs is 28.82ml (proofreading and correct the back).
Supply the computing formula of cis-propene phosphoric acid content in the test agent to be:
Claims (1)
1. cis-propene phosphoric acid content detecting method in the fosfomycin phenylethylamine calt, it is characterized in that: this detection method comprises the steps:
(1) preparation of iodine monochloride reagent: dissolving 8g iodine trichloride is in the 200ml glacial acetic acid, and dissolving 9g iodine mixes above-mentioned two kinds of solution in the 300ml glacial acetic acid, adds glacial acetic acid and is diluted to 1000ml, shakes up;
(2) preparation of starch indicator solution: get soluble starch 0.5g, after adding water 5ml and stirring, in the impouring 100ml boiling water, continued to boil 2 minutes, put coldly, get supernatant liquor;
(3) preparation of 0.1mol/L sodium thiosulfate vs: get sodium thiosulfate 26g and natrium carbonicum calcinatum 0.20g, add the cold water that newly boiled and make dissolving in right amount and be diluted to 1000ml, shake up, place the back and filter;
(4) demarcation of sodium thiosulfate vs: be taken at 120 ℃ of base weight potassium chromate 0.15g that are dried to constant weight, put in the iodine flask, add water 50ml and make dissolving, add potassium iodide 2.0g, add dilute sulfuric acid 40ml after the dissolving, shake up close plug; After in the dark placing 10 minutes, add water 250ml dilution, during with sodium thiosulfate vs titration near terminal point; Add starch indicator solution 3ml; Continue titration to blue the disappearance and show bright green, and the result of titration is proofreaied and correct with blank test, every 1ml sodium thiosulfate vs is equivalent to the potassium dichromate of 4.903mg; According to the amount of taking of the consumption and the potassium dichromate of sodium thiosulfate vs, the concentration that calculates the sodium thiosulfate vs is C mol/L;
(5) take by weighing confession test agent 2.0g; Place iodine flask, add the 20ml glacial acetic acid, add 15ml iodine monochloride reagent again; Shake up; In the dark place after 60 minutes and to add 20ml 50% potassium iodide reagents, when light yellow, the volume that writes down consume sulfur sodium thiosulfate vs is V with the titration of 0.1mol/L sodium thiosulfate vs
1Ml adds 2ml starch indicator solution, continues titration and disappears to blue, does blank test simultaneously, and the volume of record consume sulfur sodium thiosulfate vs is V
0Ml;
(6) supply the computing formula of cis-propene phosphoric acid content in the test agent to be:
V
0: the volume of blank consume sulfur sodium thiosulfate vs, ml;
V
1: sample solution consumes the volume of consume sulfur sodium thiosulfate vs, ml;
C: the concentration of sodium thiosulfate vs, mol/L;
W: the weight of test sample, mg.
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Cited By (4)
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|---|---|---|---|---|
| CN104360008A (en) * | 2014-11-07 | 2015-02-18 | 铜陵金泰化工股份有限公司 | Detection method for concentration of iodine in polyethylene glycol-potassium iodide-cyclic carbonate mixed system |
| CN109060934A (en) * | 2018-09-30 | 2018-12-21 | 东北制药集团股份有限公司 | A kind of method of palladium constituent content in detection fosfomycin phenylethylamine calt |
| CN110487955A (en) * | 2019-09-18 | 2019-11-22 | 武汉工程大学 | A kind of analysis method of technical grade cis-propene phosphoric acid |
| CN110501453A (en) * | 2019-08-16 | 2019-11-26 | 武汉工程大学 | The method for analyzing measurement technical grade cis-propene phosphoric acid content using pH meter |
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| CN101949858A (en) * | 2010-09-07 | 2011-01-19 | 长安大学 | Test method of doping quantity of modifier in SBS modified asphalt |
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| CN101949858A (en) * | 2010-09-07 | 2011-01-19 | 长安大学 | Test method of doping quantity of modifier in SBS modified asphalt |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104360008A (en) * | 2014-11-07 | 2015-02-18 | 铜陵金泰化工股份有限公司 | Detection method for concentration of iodine in polyethylene glycol-potassium iodide-cyclic carbonate mixed system |
| CN104360008B (en) * | 2014-11-07 | 2017-01-11 | 铜陵金泰化工股份有限公司 | Detection method for concentration of iodine in polyethylene glycol-potassium iodide-cyclic carbonate mixed system |
| CN109060934A (en) * | 2018-09-30 | 2018-12-21 | 东北制药集团股份有限公司 | A kind of method of palladium constituent content in detection fosfomycin phenylethylamine calt |
| CN110501453A (en) * | 2019-08-16 | 2019-11-26 | 武汉工程大学 | The method for analyzing measurement technical grade cis-propene phosphoric acid content using pH meter |
| CN110487955A (en) * | 2019-09-18 | 2019-11-22 | 武汉工程大学 | A kind of analysis method of technical grade cis-propene phosphoric acid |
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