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Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt

A technology of cis-acrylophosphate, left phosphorus and right ammonium salt, which is applied in the direction of material analysis by observing the influence on chemical indicators, and analysis by making materials undergo chemical reactions, which can solve the problems of no related reports.

Active Publication Date: 2014-01-08
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the detection method of cis-acrylophosphate content in p-left-phosphorus-right-ammonium salt

Method used

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  • Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt
  • Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt
  • Method for detecting content of cis-propenyl phophonic acid in phosphate-ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 2.0008g of the test sample, place it in a 250ml iodine bottle, add 20ml of glacial acetic acid, then precisely add 15ml of iodine monochloride reagent, cover and shake well. Leave in the dark for 60 minutes. Add 20ml of 50% potassium iodide reagent, when titrated to light yellow with sodium thiosulfate titration solution (0.09668mol / L), add 2ml of starch indicator solution, continue titration until the blue color disappears, the recorded volume is 27.30ml (after correction), and at the same time Do a blank control test, record the volume of sodium thiosulfate titration solution consumed as 28.82ml (after correction).

[0025] The formula for calculating the content of cis-acrylphosphoric acid in the test sample is:

[0026]

Embodiment 2

[0028] Weigh 2.0031g of the test sample, put it in a 250ml iodine bottle, add 20ml of glacial acetic acid, then precisely add 15ml of iodine monochloride reagent, cover and shake well. Leave in the dark for 60 minutes. Add 20ml of 50% potassium iodide reagent, when titrated to light yellow with sodium thiosulfate titration solution (0.09668mol / L), add 2ml of starch indicator solution, continue titration until the blue color disappears, the recorded volume is 27.12ml (after correction), and at the same time Do a blank control test, record the volume of sodium thiosulfate titration solution consumed as 28.82ml (after correction).

[0029] The formula for calculating the content of cis-acrylphosphoric acid in the test sample is:

[0030]

Embodiment 3

[0032] Weigh 2.0027g of the test sample, put it in a 250ml iodine bottle, add 20ml of glacial acetic acid, then precisely add 15ml of iodine monochloride reagent, cover and shake well. Leave in the dark for 60 minutes. Add 20ml of 50% potassium iodide reagent, when titrated to light yellow with sodium thiosulfate titration solution (0.09668mol / L), add 2ml of starch indicator solution, continue titration until the blue color disappears, and the recorded volume is 27.72ml (after correction), while Do a blank control test, record the volume of sodium thiosulfate titration solution consumed as 28.82ml (after correction).

[0033] The formula for calculating the content of cis-acrylphosphoric acid in the test sample is:

[0034]

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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 [0001] The invention relates to a method for detecting the content of cis-acrylphosphoric acid in left phosphorus and right amine salt in the field of drug analysis. Background technique [0002] Fosfomycin sodium [(-)-cis-1,2-epoxypropyl sodium phosphate] is a new type of broad-spectrum antibiotic, and its bactericidal mechanism is to inhibit the early synthesis of bacterial cell walls. It has been proved by clinical and pharmacological studies that phosphorus Mycin sodium has a strong bactericidal effect on most Gram-positive bacteria and Gram-negative bacteria, and can enter the cerebrospinal fluid through the blood-brain barrier. It has the advantages of no antigenicity, low toxicity, and good chemical stability. It is suitable for In internal medicine, pediatrics, ENT, urology, etc. 1R·2s-(-)-cis-1,2-epoxypropyl phosphate-R-(+)-α-phenethylamine salt, that is, left phosphorus and right amine salt, is a chemical synthesis of fosfomycin sodium. It is an i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/79
Inventor 娄玉涛孟涛尤楠金玉坤尹宏苏贵弟孟喆周岩冯文宇唐奎山刁恩德刘爱泉
Owner NORTHEAST PHARMA GRP