A kind of liquid chromatography method for determination of clavulanate related substances in amoxicillin clavulanate potassium pharmaceutical composition

A technology of potassium amoxicillin-clavulanate and potassium clavulanate, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as interference, improve accuracy, achieve accurate and reliable results, and facilitate product quality control Effect

Active Publication Date: 2022-07-26
JIANGSU SIMCERE PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed determination method of related substances of clavulanic acid is HPLC method (see Chinese Pharmacopoeia 2015 Edition Part Two), and it is found through research that during the experimental operation, the above method is easily affected by the main component amoxicillin and other impurities in the pharmaceutical composition. interference

Method used

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  • A kind of liquid chromatography method for determination of clavulanate related substances in amoxicillin clavulanate potassium pharmaceutical composition
  • A kind of liquid chromatography method for determination of clavulanate related substances in amoxicillin clavulanate potassium pharmaceutical composition
  • A kind of liquid chromatography method for determination of clavulanate related substances in amoxicillin clavulanate potassium pharmaceutical composition

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Experimental equipment and conditions:

[0065] Agilent high performance liquid chromatograph; DAD detector; Waters Atlantis T3, 5μm, 250×4.6mm as the separation column.

[0066] Detection conditions:

[0067] Flow rate: 1.0ml / min; Detection wavelength: 214nm; Column temperature: 30℃; Injection volume: 20μl; Mobile phase A: 0.03mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid); Mobile phase B: 0.03mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20), carry out linear gradient elution according to Table 1:

[0068] Table 1 Gradient elution procedure

[0069]

[0070] Experimental procedure: 0.03mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid) as mobile phase A, use 0.03mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20) It is mobile phase B, eluted according to the gradient in Table 1, the ...

Embodiment 2

[0073] Experimental equipment and conditions:

[0074] Agilent high performance liquid chromatograph; DAD detector; Waters Atlantis T3, 5μm, 250×4.6mm as the separation column.

[0075] Detection conditions:

[0076] Flow rate: 0.8ml / min; Detection wavelength: 214nm; Column temperature: 30℃; Injection volume: 20μl; Mobile phase A: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid); Mobile phase B: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20), carry out linear gradient elution according to Table 2:

[0077] Table 2 Gradient elution procedure

[0078]

[0079]

[0080] Experimental procedure: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid) as mobile phase A, use 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20) It is mobile phase B, eluted according to the gradient in T...

Embodiment 3

[0083] Experimental equipment and conditions:

[0084] Agilent high performance liquid chromatograph; DAD detector; Waters Atlantis T3, 5μm, 250×4.6mm as the separation column.

[0085] Detection conditions:

[0086] Flow rate: 1.2ml / min; Detection wavelength: 214nm; Column temperature: 30℃; Injection volume: 20μl; Mobile phase A: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid); Mobile phase B: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20), carry out linear gradient elution according to Table 3:

[0087] Table 3 Gradient elution procedure

[0088]

[0089] Experimental procedure: 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid) as mobile phase A, use 0.05mol / L ammonium acetate aqueous solution (adjust pH to 5.70 with glacial acetic acid)-acetonitrile (80:20) It is mobile phase B, eluted according to the gradient in Table 3, the ...

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Abstract

The invention discloses a liquid chromatography method for the determination of clavulanate related substances in a pharmaceutical composition of amoxicillin-clavulanate potassium. The method uses octadecylsilane-bonded silica gel as filler and ammonium acetate aqueous solution as mobile phase A, ammonium acetate aqueous solution-acetonitrile is mobile phase B, and linear gradient elution is performed, and the pH value of the ammonium acetate aqueous solution is 5.60-5.80. The method provided by the invention can effectively detect the clavulanic acid impurities in the amoxicillin clavulanate potassium pharmaceutical composition, has high separation degree, is simple and easy to implement, has low analysis cost, accurate and reliable results, and is convenient for production and quality control of products in the process quality control.

Description

technical field [0001] The invention belongs to the field of drug impurity analysis and detection, in particular to a liquid chromatography method for determining the related substances of clavulanate in amoxicillin clavulanate potassium pharmaceutical composition. Background technique [0002] Amoxicillin is one of the most commonly used broad-spectrum β-lactam antibiotics, which has strong bactericidal effect and ability to penetrate cell membranes, but is unstable to β-lactamase. Clavulanic acid is an irreversible competitive β-lactamase inhibitor. The combination of the two can protect amoxicillin from β-lactamase hydrolysis and significantly enhance the antibacterial effect of amoxicillin. It is widely used in the treatment of various infectious diseases clinically. [0003] The chemical structural formula of Clavulanate Potassium is: [0004] [0005] It is known in the art that potassium clavulanate is chemically unstable, and is easily degraded during production...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor江玉婷李雯杨文玲薛其俊吴暎李薇任晋生
OwnerJIANGSU SIMCERE PHARMA