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An analysis method for measuring related substances in diclofenac sodium raw materials and preparations thereof

A technology for diclofenac sodium and related substances is applied in the analysis field of measuring diclofenac sodium raw materials and related substances in preparations thereof, and can solve the problems of inability to accurately and effectively measure the content of impurity D, affecting the recovery rate of impurity D, poor separation of diclofenac sodium, and the like, Achieve reliable quality control methods, improved recovery, and improved resolution

Pending Publication Date: 2020-01-14
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the current quality standards and the high performance liquid chromatography conditions under the relevant substances of diclofenac sodium raw materials and preparations thereof in the European Pharmacopoeia, the separation of impurity D and diclofenac sodium is poor, which seriously affects the recovery rate of impurity D
Under the ultra-high performance liquid chromatographic conditions under the related substances of the United States Pharmacopoeia Diclofenac Sodium Sustained-release Tablets, the relative retention time of impurity D is 1.04, which is poorly separated from the main peak, and the recovery rate is only 76%, which cannot accurately and effectively measure the content of impurity D. content

Method used

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  • An analysis method for measuring related substances in diclofenac sodium raw materials and preparations thereof
  • An analysis method for measuring related substances in diclofenac sodium raw materials and preparations thereof
  • An analysis method for measuring related substances in diclofenac sodium raw materials and preparations thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] UPLC conditions:

[0039] The chromatographic column is octadecylsilane-bonded silica gel column YMC-Triart (2.0mm×100mm, 1.9um), with acetonitrile as mobile phase A, and 0.7708g / L ammonium acetate solution (adjusted to pH 5.3 with acetic acid) as mobile phase In phase B, the detection wavelength is 254 nm, the flow rate is 0.3 ml / min, and the column temperature is 35 °C, and gradient elution is performed. The gradient elution procedure is shown in Table 2.

[0040] Table 2 Gradient elution program table

[0041]

[0042] Sample preparation:

[0043] System suitability solution: Weigh appropriate amounts of diclofenac sodium reference substance and impurity A, B, C, D, E, F reference substance respectively, accurately weigh, dissolve and dilute with 50% acetonitrile to prepare each 1ml containing approximately diclofenac The mixed solution of 1 mg of sodium and impurities A, B, C, D, E, and F is 2 μg as the system suitability solution.

[0044] Test solution: take...

Embodiment 2

[0049]Ultra-high performance liquid chromatography conditions: the same as in Example 1.

[0050] Sample preparation:

[0051] System suitability solution: same as Example 1.

[0052] Test solution: Take 20 diclofenac sodium sustained-release tablets (specification: 100mg), grind and mix well, take an appropriate amount of fine powder (equivalent to about 50mg of diclofenac sodium), accurately weigh it, put it in a 50ml measuring bottle, add 50% acetonitrile About 35ml, ultrasonic for 25min, dilute to the mark with 50% acetonitrile, shake well, centrifuge, take the supernatant and filter it with 0.45μm filter membrane, take the filtrate as the test solution.

[0053] Reference substance solution: Take an appropriate amount of diclofenac sodium reference substance, accurately weigh it, dissolve it with 50% acetonitrile and quantitatively dilute it to make a solution containing about 1 μg of diclofenac sodium per 1 ml, as the reference substance solution.

[0054] Determinatio...

Embodiment 3

[0057] Ultra-high performance liquid chromatography conditions: the same as in Example 1.

[0058] Sample preparation:

[0059] Precisely weigh impurity A 10.06 mg, impurity B 10.53 mg, impurity C 10.31 mg, impurity D 9.65 mg, impurity E 10.20 mg, impurity F 9.85 mg, and diclofenac sodium 10.01 mg, respectively, put them in 25ml measuring flasks, dissolve 50% acetonitrile, Dilute to the mark, shake well, and use it as the stock solution for each reference substance. Accurately measure an appropriate amount of each reference substance stock solution, dilute it with 50% acetonitrile to prepare a series of solutions, and precisely measure 1 μl according to the chromatographic conditions of Example 1, inject it into a liquid chromatograph, and record the chromatogram. Taking the concentration (μg / ml) as the X-axis and the peak area as the Y-axis, the linear regression equation and correction factor (ratio of the slope of diclofenac sodium to the slope of each impurity) of each co...

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Abstract

The invention discloses an analysis method for measuring related substances in diclofenac sodium raw materials and preparations thereof. The method adopts ultra-high-performance liquid chromatography;and the chromatographic conditions are as follows: a chromatographic column is an octadecylsilane chemically bonded silica gel chromatographic column; and gradient elution is carried out with acetonitrile being as a mobile phase A, an ammonium acetate solution being as a mobile phase B and the detection wavelength being 254nm. The method can accurately and efficiently measure the content of an impurity D in the diclofenac sodium raw materials and the preparations thereof, and meanwhile, can measure the existence and / or content of impurities A, B, C, E and F.

Description

technical field [0001] The invention relates to the technical field of chemical drug analysis methods, in particular to an analysis method for determining diclofenac sodium raw materials and related substances in preparations thereof. Background technique [0002] Diclofenac Sodium, the chemical name is 2-[(2,6-dichlorophenyl)amino]-phenylacetate, and its molecular formula is C 14 H 10 Cl 2 NNaO 2 , the molecular weight is 318.13, and its structural formula is as follows: [0003] [0004] Diclofenac sodium is an antipyretic analgesic, non-steroidal anti-inflammatory drug, suitable for relieving rheumatoid arthritis, osteoarthritis, spondyloarthropathy, gouty arthritis, rheumatoid arthritis, etc. Impurity D (2-(2-bromo-6-chlorophenylamino)phenylacetic acid) is a by-product in the synthesis process of diclofenac sodium, and exists in the raw materials of diclofenac sodium and its preparation; the long-term stability test results of diclofenac sodium sustained-release t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/86
CPCG01N30/02G01N30/34G01N30/8631
Inventor 王静刘燕刘彩霞杨琪刘亚方杨帅
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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