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Method for detecting content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography

A kind of headspace gas chromatography, levophosphine dexamine salt technology, applied in the field of drug analysis

Active Publication Date: 2018-01-19
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching the literature, there is currently no relevant report on the detection of the residual propynyl alcohol in the left phosphorus and right ammonium salt. Therefore, a simple, time-saving and suitable detection method for real-time monitoring of the content of propynyl alcohol in the left phosphorus and right ammonium salt is developed. New issues to be solved urgently

Method used

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  • Method for detecting content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography
  • Method for detecting content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography
  • Method for detecting content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Instrument conditions:

[0025] Chromatographic column: DB-1301 30m×0.53mm×1μm (capillary packed column filled with 6% cyanopropyl and 94% methylpolysiloxane, manufacturer: Agilent);

[0026] Detector: flame ionization detector;

[0027] Carrier gas: N2;

[0028] Column temperature: The initial column temperature of the instrument should be 70°C for 5 minutes, then raise the temperature to 115°C at 10°C / min and hold for 1 minute, then raise the temperature to 200°C at 50°C / min and hold for 2 minutes;

[0029] Headspace bottle press time is 0.05min;

[0030] The column flow rate is 4ml / min;

[0031] Injection volume: 1ml;

[0032] (2) Preparation of system adaptability solution:

[0033] Accurately weigh 0.5052 g of propynyl alcohol in a 100 ml volumetric flask, and add water to make up to the mark. Then accurately draw 1.0ml of this solution into a 200ml volumetric flask, and add water to make up to the mark.

[0034] (3) Preparation of the test solution:

...

Embodiment 2

[0047] Establishment of methodology

[0048] 1 specificity test

[0049] 1.1 Preparation of system suitability solution:

[0050] Accurately weigh an appropriate amount of propynyl alcohol, add water to dissolve and dilute;

[0051] 1.2 Precisely measure 10ml of solvent water and system suitability test solution into a 20ml headspace bottle and seal it immediately; record the chromatogram, which shows that there is no interference from solvent water.

[0052] 2 linear range

[0053] Accurately weigh 0.5 g of propynyl alcohol in a 100 ml volumetric flask, add water to make up to the mark. Then accurately draw 1.0ml of this solution into a 200ml volumetric flask, and add water to make up to the mark.

[0054] Precisely measure 0.1, 0.25, 0.5, 1.0ml, and 1.2ml of the above solution into five 200ml volumetric flasks, dilute with water to the mark, shake well, precisely measure 10ml of the above solution into a 20ml headspace bottle, and seal it immediately; Record the chromat...

Embodiment 3

[0070] 1. Selection of chromatographic column

[0071] The chromatographic column filled with 6% cyanopropyl and 94% methyl polysiloxane has the best peak shape of propargyl alcohol, the best tailing factor, the best repeatability and durability of the method.

[0072] 2. Selection of headspace bottle press time

[0073] Adjust the headspace bottle pressure time to 0.05min.

[0074] 3. Selection of instrument column temperature

[0075] The initial column temperature of the instrument should be 70°C and kept for 5 minutes to make the main peak come out, then increase the temperature at 10°C / min to 115°C and hold for 1 minute, then increase the temperature to 200°C at 50°C / min and keep for 2 minutes to remove all impurity peaks.

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Abstract

Belonging to the field of pharmaceutical analysis, the invention relates to a method for detecting the content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography. The method includes the steps of: (1) preparing the instrument conditions: adopting a capillary packed column using cyanopropyl and methylpolysilicone as the filler as the chromatographic column;(2) preparing a system adaptive solution; (3) preparing a test solution; and (4) performing testing: putting the system adaptive solution into a headspace sample injector, recording the spectrogram,calculating the propargyl alcohol peak area's relative standard deviation RSD that is less than or equal to 10.0%, precisely weighing the test solution and putting it into the headspace sample injector, recording the spectrogram, and calculating the content of propargyl alcohol in phosphonomycin-1-phenethylamine salt. The method provided by the invention has the advantages of good propargyl alcohol separation effect, good method repeatability and durability, good peak reproducibility, good peak shape, simple operation, time saving, high efficiency and the like.

Description

technical field [0001] The invention relates to a method for detecting the content of propynyl alcohol in left phosphorus and right amine salts by headspace gas chromatography in the field of drug analysis. Background technique [0002] Fosfomycin has antibacterial effect on Gram-positive cocci such as Staphylococcus aureus and Staphylococcus epidermidis, and has antibacterial effect on Escherichia coli, Serratia, Shigella, Yersinia, Pseudomonas aeruginosa, pneumoniae Gram-negative bacteria such as Lebsiella, Enterobacter aerogenes, Vibrio and Aeromonas also have strong antibacterial activity. Fosfomycin can inhibit the early synthesis of bacterial cell walls, and its molecular structure is similar to that of phosphoenolpyruvate, so it can compete with bacteria for the same transferase, inhibiting bacterial cell wall synthesis and leading to bacterial death. [0003] Levophosphorylamine salt is the starting material for the production of fosfomycin sodium, and the starting ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 辛潇邵冬梅刘晨芳赵明冯文宇周秀峰任赫娄玉涛扬琳谢丹唐奎山
Owner NORTHEAST PHARMA GRP
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