Method for detecting chloroacetyl chloride in diclofenac sodium

A technology of diclofenac sodium and chloroacetyl chloride, applied in the directions of measuring devices, instruments, scientific instruments and the like

Active Publication Date: 2021-08-06
珠海润都制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no published method for detecting the content of chloroacetyl chloride in diclofenac sodium, especially the detection of ultra-trace amounts of chloroacetyl chloride

Method used

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  • Method for detecting chloroacetyl chloride in diclofenac sodium
  • Method for detecting chloroacetyl chloride in diclofenac sodium
  • Method for detecting chloroacetyl chloride in diclofenac sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Preparation solution: blank solution: methanol;

[0048] Reference solution: take a 100ml volumetric flask, accurately weigh about 150mg of the chloroacetyl chloride reference substance, put it in the bottle, add blank solution to dilute to the mark, and shake well; take a 100ml volumetric flask, precisely measure 10.0ml of the above solution, put it in the bottle , add blank solution to dilute to the mark, and shake well; take a 100ml volumetric flask, accurately measure 1.0ml of the above solution, put it in the bottle, add blank solution to dilute to the mark, and shake well. (Concentration: 1.5μg / ml)

[0049] Test solution: Take a 10ml volumetric flask, accurately weigh about 2g of diclofenac sodium sample, put it in the bottle, add blank solution to dissolve and dilute to the mark, and shake well. (Concentration: 0.2g / ml)

[0050] (2) Chromatographic conditions:

[0051] Instrument: gas chromatograph with FID detector, automatic sample injector, electronic a...

Embodiment 2

[0066] Example 2: System Suitability

[0067] The system suitability is realized by measuring the RSD of the peak area of ​​chloroacetyl chloride in the 5-pin reference solution, and it is required that the RSD of the peak area of ​​chloroacetyl chloride in the 5-pin reference solution should be ≤10.0%.

[0068]

Embodiment 3

[0069] Example 3: Specificity

[0070] The specificity of the method is achieved by determining whether the blank solvent interferes with the detection of chloroacetyl chloride; the separation between chloroacetyl chloride and adjacent peaks in the selective solution. It is required that the blank solvent should not interfere with the detection of chloroacetyl chloride; the separation between chloroacetyl chloride and adjacent peaks in the selective solution should be ≥ 1.5.

[0071]

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PUM

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Abstract

The invention belongs to the technical field of pharmaceutical analysis, particularly relates to a method for detecting chloracetyl chloride in diclofenac sodium, and provides a convenient, efficient and accurate detection method for solving the problem of detection of chloracetyl chloride in diclofenac sodium, the method can be used for detecting the content of chloracetyl chloride in diclofenac sodium so as to effectively guarantee the medication safety, and the quality control of diclofenac sodium API can be conveniently controlled. The method is convenient, efficient and accurate, the system applicability, repeatability, specificity and accuracy completely conform to the guidance principle verified by the method in the Chinese pharmacopoeia, and the method can be used for quality control of the diclofenac sodium bulk drug.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for testing chloroacetyl chloride in diclofenac sodium. Background technique [0002] Diclofenac Sodium (Diclofenac Sodium), the chemical name is 2-[(2,6-dichlorophenyl)amino]-sodium phenylacetate, and its molecular formula is C 14 h 10 C l2 NNaO 2 , the molecular weight is 318.13, and its structural formula is as follows: Diclofenac sodium is an antipyretic and analgesic, non-steroidal anti-inflammatory drug, suitable for relieving rheumatoid arthritis, osteoarthritis, spondyloarthropathy, gouty arthritis, rheumatoid arthritis, etc. Chloroacetyl chloride is diclofenac The by-product in the sodium synthesis process exists in the raw material of diclofenac sodium. Chloroacetyl chloride has a warning structural group and is a potential genotoxic impurity, which may have genotoxicity and carcinogenicity. In order to ensure the safety and effectiveness of the drug...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/68G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/68G01N30/8675G01N2030/324
Inventor 蔡强吴挺强谢金昌汤伟彬兰柳琴
Owner 珠海润都制药股份有限公司
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