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Method for determining related substances in fosfomycin sodium by using nuclear magnetic resonance hydrogen spectrum

A technology of proton nuclear magnetic resonance spectroscopy and related substances, which is applied to the analysis of nuclear magnetic resonance, can solve the problems of long analysis time, loss of water-soluble components, loss of chromatographic separation, etc., and achieves simple operation, rapid measurement and good reproducibility Effect

Pending Publication Date: 2022-01-11
广东利玮医药有限公司
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  • Abstract
  • Description
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Problems solved by technology

[0006] The above two high-performance liquid chromatography methods for determining the related substances of fosfomycin sodium have good versatility and specificity for specific impurities, and are easy to operate, but there are still the following defects: ① Chromatographic separation loss: commonly used ODS chromatographic columns are lost during the separation process. Water-soluble components with high polarity are lost in medium; ②The analysis time is longer

Method used

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  • Method for determining related substances in fosfomycin sodium by using nuclear magnetic resonance hydrogen spectrum
  • Method for determining related substances in fosfomycin sodium by using nuclear magnetic resonance hydrogen spectrum
  • Method for determining related substances in fosfomycin sodium by using nuclear magnetic resonance hydrogen spectrum

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Embodiment 1

[0063] (1Z)-prop-1-en-1-yl phosphonate sodium, propyl phosphonate sodium, 2-propenyl phosphonate sodium and (1,2-dihydroxypropyl ) The mensuration of sodium phosphonate comprises the following steps:

[0064] The first step: the preparation of the first mixed solution: Accurately weigh 470.5 mg of fosfomycin sodium sample II with a mass fraction of 99.3% and 190.1 mg of 4-bromopyridine hydrochloride with a mass fraction of 90%, dissolve in 10 ml D 2 O, the first mixed solution was obtained;

[0065] Step 2: Preparation of test solution: Accurately measure 0.5ml of the first mixed solution, add 10ml of D 2 O is diluted to obtain the test solution (the test solution containing 23.36mg fosfomycin sodium and 8.55mg mass fraction is 90% 4-bromopyridine hydrochloride);

[0066] The third step: proton nuclear magnetic resonance spectrum test: the test procedure is the same as that of the blank control example. Record the spectrum. The internal standard and the characteristic peak...

Embodiment 2

[0077] (1Z)-prop-1-en-1-yl phosphonate sodium, propyl phosphonate sodium, 2-propenyl phosphonate sodium and (1,2-dihydroxypropyl ) The mensuration of sodium phosphonate comprises the following steps:

[0078] The first step: the preparation of test solution: accurately measure the first mixed solution 0.5ml in embodiment one, add 10mlD 2 O is diluted to obtain the second mixed solution; adding 0.1ml to the second mixed solution containing 20ml of propylphosphonic acid 10.1mg with a mass fraction of 95% 2 O solution, to get the test solution (the test solution containing 23.36mg fosfomycin sodium and 8.55mg mass fraction is 90% 4-bromopyridine hydrochloride);

[0079] The remaining steps are the same as in Embodiment 1.

[0080] The amount of propylphosphonic acid with a mass fraction of 95% in the test solution of Example 2 is 0.05 mg.

[0081] In the second embodiment 1 H NMR spectrum as Figure 4 shown.

Embodiment 3

[0083] (1Z)-prop-1-en-1-yl phosphonate sodium, propyl phosphonate sodium, 2-propenyl phosphonate sodium and (1,2-dihydroxypropyl ) The mensuration of sodium phosphonate comprises the following steps:

[0084] The first step: the preparation of test solution: accurately measure the first mixed solution 0.5ml in embodiment one, add 10mlD 2 O is diluted to obtain the second mixed solution; in the second mixed solution, adding 0.2ml containing 20ml of propylphosphonic acid 10.1mg with a mass fraction of 95% 2 O solution, to get the test solution (the test solution containing 23.36mg fosfomycin sodium and 8.55mg mass fraction is 90% 4-bromopyridine hydrochloride);

[0085] The remaining steps are the same as in Embodiment 1.

[0086] The amount of propylphosphonic acid with a mass fraction of 95% in the test solution of Example 3 was 0.10 mg.

[0087] In the third embodiment 1 H NMR spectrum as Figure 5 shown.

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Abstract

The invention discloses a method for determining related substances in fosfomycin sodium by using the hydrogen nuclear magnetic resonance spectroscopy. The method adopted by the invention is a nuclear magnetic resonance hydrogen spectrum method, preferably, 4-bromopyridine hydrochloride is used as an internal standard substance, more preferably, 4-bromopyridine hydrochloride with the mass fraction of 90% is used as the internal standard substance, and D2O is selected as a deuterated solvent. The method for determining related substances in fosfomycin sodium comprises the following specific steps: (1) precisely weighing a fosfomycin sodium certification batch sample and an internal standard substance, and dissolving thefosfomycin sodium certification batch sample and the internal standard substance in a deuterated solvent to obtain a test solution; (2) precisely measuring the test solution, transferring the test solution into an NMR (nuclear magnetic resonance) tube, performing a nuclear magnetic resonance hydrogen spectrum test, and recording a spectrogram, wherein the conditions of the nuclear magnetic resonance hydrogen spectrum test comprise: a Bruker DRX300 nuclear magnetic resonance spectrometer equipped with a 5mm multi-core QNP probe; the frequency spectrum width is 3500Hz; the temperature is 296 K; the pulse is 30 degrees; the acquisition time is 4.7 s; and the deuterated solvent is D2O. The determination method disclosed by the invention is simple and easy to implement, high in accuracy and strong in specificity, and can well control impurities in a sample and ensure the quality of the sample.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for determining related substances in fosfomycin sodium by using hydrogen nuclear magnetic resonance spectroscopy. Background technique [0002] Fosfomycin is structurally a phosphoric acid derivative, a new type of broad-spectrum antibiotic discovered and developed in 1967 by Merck and CEPA in Spanish soil in Streptomyces. Mainly used for Gram-negative and positive bacterial infections. [0003] Fosfomycin sodium and calcium salts were launched in Europe in 1975; Meiji products were launched in Japan in 1980; fosfomycin butanetriol was launched in Europe in 1988; and in the United States in 1996. The main dosage form of fosfomycin is fosfomycin sodium powder injection, which is suitable for infusion and intravenous injection. Other dosage forms include fosfomycin calcium tablets, capsules, syrup, etc. At present, there are mainly 4 varieties of fosfomycin, namel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 陈丹
Owner 广东利玮医药有限公司
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