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Method for detecting methyl acetoacetate in cefradine

A technology of methyl acetoacetate and cefradine is applied in the detection field of methyl acetoacetate, a related substance in cefradine, and can solve the problems of low sensitivity, large error in the content determination result of reversed-phase high performance liquid chromatography, poor peak shape and the like , to achieve high sensitivity, easy product quality control, and accurate quantitative results

Inactive Publication Date: 2020-09-11
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) the ultraviolet absorption of methyl acetoacetate is very weak, adopts the reversed-phase high performance liquid chromatography detection method detection of cephradine related substance in the Pharmacopoeia, and sensitivity is low;
[0008] (2) Methyl acetoacetate chromatographic peak tailing is serious, and peak shape is poor, and assay result is inaccurate, when being used for the quality control of cefradine in the large-scale production process, reversed-phase high performance liquid chromatography assay result error is bigger

Method used

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  • Method for detecting methyl acetoacetate in cefradine
  • Method for detecting methyl acetoacetate in cefradine
  • Method for detecting methyl acetoacetate in cefradine

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Experimental equipment and chromatographic conditions:

[0034] Instrument: Shimadzu GC-2010Pro gas chromatograph;

[0035] Chromatographic column: Agilent HP-INNOWAX (30m×0.530mm, 1.0μm, SN: USP465141H);

[0036] Column temperature: The initial column temperature is 40°C, maintained for 6 minutes, and raised to 150°C at a rate of 20°C per minute, maintained for 12 minutes;

[0037] Injection port temperature: 200°C;

[0038] Split ratio: 10;

[0039] Hydrogen flame ionization detector temperature: 250°C;

[0040] Carrier gas (nitrogen) flow rate: 5.0ml / min;

[0041] Injection volume: 1 μl.

[0042] Implementation steps:

[0043] Solution preparation: use water as a blank solution; accurately weigh an appropriate amount of methyl acetoacetate, dissolve and dilute with water to make a solution with a concentration of about 100 μg / ml, use it as a stock solution of methyl acetoacetate reference substance, and then precisely measure 1.0ml, Put in 10ml measuring bottl...

Embodiment 2

[0049] Experimental equipment and chromatographic conditions:

[0050] Instrument: Shimadzu GC-2010Pro gas chromatograph;

[0051] Chromatographic column: Agilent HP-INNOWAX (30m×0.530mm, 1.0μm, SN: USP465141H);

[0052] Column temperature: The initial column temperature is 40°C, maintained for 6 minutes, and raised to 150°C at a rate of 20°C per minute, maintained for 12 minutes;

[0053] Injection port temperature: 200°C;

[0054] Split ratio: 10;

[0055] Hydrogen flame ionization detector temperature: 250°C;

[0056] Carrier gas (nitrogen) flow rate: 4.8ml / min;

[0057] Injection volume: 1 μl.

[0058] Implementation steps:

[0059] Solution preparation: use water as a blank solution; accurately weigh an appropriate amount of methyl acetoacetate, dissolve and dilute with water to make a solution with a concentration of about 100 μg / ml, use it as a stock solution of methyl acetoacetate reference substance, and then precisely measure 1.0ml, Put in 10ml measuring bottl...

Embodiment 3

[0065] Experimental equipment and chromatographic conditions:

[0066] Instrument: Shimadzu GC-2010Pro gas chromatograph;

[0067] Chromatographic column: Agilent HP-INNOWAX (30m×0.530mm, 1.0μm, SN: USP465141H);

[0068] Column temperature: The initial column temperature is 40°C, maintained for 6 minutes, and raised to 150°C at a rate of 20°C per minute, maintained for 12 minutes;

[0069] Injection port temperature: 200°C;

[0070] Split ratio: 10;

[0071] Hydrogen flame ionization detector temperature: 250°C;

[0072] Carrier gas (nitrogen) flow rate: 5.2ml / min;

[0073] Injection volume: 1 μl.

[0074] Implementation steps:

[0075] Solution preparation: use water as a blank solution; accurately weigh an appropriate amount of methyl acetoacetate, dissolve and dilute with water to make a solution with a concentration of about 100 μg / ml, use it as a stock solution of methyl acetoacetate reference substance, and then precisely measure 1.0ml, Put in 10ml measuring bottl...

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Abstract

The invention provides a method for detecting impurity methyl acetoacetate in cefradine. A GC external standard method is adopted to qualitatively and quantitatively analyze methyl acetoacetate in cefradine, experimental operation is simple, water is used as a solvent in the analysis and detection process, pollution is avoided, chromatographic peaks are free of interference, peak patterns are symmetrical, methodological verification results all meet requirements, and it is shown that the detection method is good in specificity, high in sensitivity and accurate in quantification. The detectionmethod provided by the invention is suitable for detection of methyl acetoacetate in cefradine, and is convenient for large-scale production and control of product quality in a quality control process.

Description

technical field [0001] The invention belongs to the field of drug impurity detection, in particular to a method for detecting methyl acetoacetate, a related substance in cephradine. Background technique [0002] Cephradine chemical name: (6R,7R)-7-[(R)-2-amino-2-(1,4-cyclohexadien-1-yl)acetamido]-3-methyl-8-oxo -5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, molecular formula: C 16 h 19 N 3 o 4 S, molecular weight: 349.40. Its structural formula is: [0003] [0004] Cefradine is a β-lactam antibiotic, used for acute pharyngitis, tonsillitis, otitis media, bronchitis and pneumonia and other respiratory tract infections, urogenital tract infections and skin and soft tissue infections caused by sensitive bacteria. In order to ensure the quality and efficacy of cephradine, it is very necessary to carry out the detection and control of related substances. [0005] At present, ChP, USP, BP and other national pharmacopoeias have recorded the detection methods of ...

Claims

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Application Information

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IPC IPC(8): G01N30/68G01N30/06
CPCG01N30/06G01N30/68
Inventor 王付荣吴辉李丹
Owner SHANDONG XINHUA PHARMA CO LTD
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