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Method for detecting polymers in cefotaxime sodium and injection thereof

A technology of cefotaxime and thioxime sodium, which is applied in the field of rapid determination of polymer content in cefotaxime sodium drugs, can solve the problems of low column efficiency and long analysis time, and achieve high accuracy, good repeatability, and linearity wide range of effects

Inactive Publication Date: 2018-11-23
江苏省食品药品监督检验研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the chromatographic columns used in this method are self-packed, with low column efficiency and long analysis time

Method used

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  • Method for detecting polymers in cefotaxime sodium and injection thereof
  • Method for detecting polymers in cefotaxime sodium and injection thereof
  • Method for detecting polymers in cefotaxime sodium and injection thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Determination of polymer content in cefotaxime sodium and its injection by external standard method.

[0021] 1.1 Chromatographic conditions

[0022] Chromatographic column: a chromatographic column (SRTSEC-150, 7.8*300mm, 5μm) filled with a spherical silica gel matrix bonded to the surface of a nano-neutral hydrophilic film; mobile phase: 0.1mol / L phosphate buffer [0.1mol / L phosphoric acid Disodium hydrogen-0.1mol / L sodium dihydrogen phosphate solution (61:39)]; flow rate: 0.8mL / min; detection wavelength: 235nm. Injection volume: 10 μL. Column temperature: 35°C.

[0023] 1.2 Experimental steps

[0024] Preparation of reference solution

[0025] Take an appropriate amount of cefotaxime reference substance, accurately weigh it, add water to dissolve and quantitatively dilute to make a solution containing about 10 μg of cefotaxime sodium in every 1 ml, to obtain the product.

[0026] Preparation of the test solution

[0027] Take an appropriate amount of t...

Embodiment 2

[0044] The identification of each impurity peak of embodiment 2

[0045] 2.1 Impurities with impurity reference substances: (A, B, E) (impurities 6, 5, 8)

[0046] Using cefotaxime existing reference substance cefotaxime impurity A (deacetyl cefotaxime), cefotaxime impurity B (deacetyl cefotaxime), cefotaxime impurity E (deacetyl cefotaxime lactone ) for sample injection analysis, impurity 6, 5, and 8 are respectively consistent with impurity A, B, E retention time in the chromatogram of need testing solution.

[0047] 2.2 Impurities of the reference substance without impurities: (impurities 1, 2, 3, 4, 7)

[0048]2.2.1 Chromatography and mass spectrometry conditions The chromatographic conditions are 0.02mol / L ammonium acetate as the mobile phase, the detection wavelength is 235nm, the column temperature is 35°C, and the flow rate is 0.3mL / min. Packed chromatographic column (SRT SEC-150, 7.8*300mm, 5μm).

[0049] Mass Spectrometry Conditions Electrospray ionization source ...

Embodiment 3

[0054] Embodiment 3 The typical chromatogram comparison of the inventive method and " Chinese Pharmacopoeia " 2015 edition cefotaxime sodium polymer method

[0055] 3.1 "Chinese Pharmacopoeia" 2015 edition cefotaxime polymer Sephadex G10 gel chromatography conditions

[0056] "Chinese Pharmacopoeia" 2015 edition cefotaxime polymer Sephadex G10 gel chromatography salt phase: 0.1mol / L phosphate buffer [0.1mol / L disodium hydrogen phosphate-0.1mol / L sodium dihydrogen phosphate (61:39 )], detection wavelength: 254nm; injection volume 100μl. Sample concentration: 20mg / ml, the typical chromatogram obtained is as attached Figure 5 , the polymer impurity peak is enriched, and the method of the present invention is used for reanalysis, and the results are as attached Figure 6 , show that the method of the present invention has better separation ability, obtain 4 impurity peaks before main peak cefotaxime, and No. 1, 2, 3 and No. 4 peaks obtained by separation of the aforementioned n...

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Abstract

The invention belongs to the field of pharmaceutical analysis, and relates to a method for determining polymers in cefotaxime sodium and an injection thereof. The invention adopts high performance liquid chromatography and an external standard method to determine the content of polymers in cefotaxime sodium-like drugs. The chromatographic conditions are as follows: adopting a chromatographic column with spherical silica gel matrix with the surface bonded with a nano-hydrophilic film is used as a filler, taking 0.1 mol / L phosphate buffer solution [0.1 mol / L disodium hydrogen phosphate-0.1 mol / Lsodium dihydrogen phosphate solution (61:39)] is used as a mobile phase, the flow rate is 0.8 mL / min, the detection wavelength is 235 nm, the injection amount: is 10 muL, and the column temperature:is 35 DEG C. The method has the advantages of a wide linear range, high accuracy, good repeatability and the like, and overcomes the disadvantages of poor reproducibility of the sephadex method, long analysis time, poor separation ability, incapability of accurately determining the content of a single polymer and the like of the sephadex method.

Description

technical field [0001] The invention relates to the field of drug analysis, and specifically provides a method for rapidly determining the polymer content in cefotaxime sodium drugs. Background technique [0002] Cefotaxime sodium is a semi-synthetic third-generation cephalosporin antibiotic, which belongs to the β-lactam antibiotics and has good antibacterial effects on both Gram-negative bacteria and Gram-positive bacteria. Its clinical adverse reactions include anaphylactic shock, acute angioneurotic edema, drug fever, allergic asthma and systemic allergy. Anaphylaxis is the most concerned adverse reaction of β-lactam antibiotics, and it has been reported that high molecular polymer impurities are the main cause of anaphylaxis. Polymer impurities are divided into endogenous impurities and exogenous impurities. Endogenous impurities refer to oligomers or polymers produced by the polymerization of antibiotics themselves. Exogenous impurities are usually polysaccharides, pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74G01N30/72
CPCG01N30/02G01N30/72G01N30/74
Inventor 袁耀佐侯玉荣张玫赵丽丽赵述强杭太俊樊夏雷
Owner 江苏省食品药品监督检验研究院
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