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Method for detecting specific impurities of mesalazine

A detection method, the technology of mesalazine, which is applied in the field of medicine, can solve the problems of small amount of specific impurities, high operation requirements, and high instrument requirements, and achieve the effects of strong specificity, good precision, and high sensitivity

Inactive Publication Date: 2018-06-15
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The number of specific impurities controlled in the existing national drug standards and US drug standards is small, which cannot meet the requirements for improving drug quality
The gradient elution method used in the European Pharmacopoeia and the British Pharmacopoeia has high requirements on the instrument and the operation. It is often necessary to adjust the gradient conditions when replacing the instrument. Effective separation between specific impurities and specific impurities, and no inspection and control of hydroquinone and p-benzoquinone

Method used

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  • Method for detecting specific impurities of mesalazine
  • Method for detecting specific impurities of mesalazine
  • Method for detecting specific impurities of mesalazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Using a phenyl-bonded silica gel column, the mobile phase is the aqueous phase (1.36g potassium dihydrogen phosphate and 1.73g sodium octane sulfonate, dissolved in 890ml water, add phosphoric acid to adjust the pH to 2.00)-methanol-acetonitrile-tetrahydrofuran (890 :58:34:18), the flow rate is 1.2ml / min, the detection wavelength is 220nm, and the column temperature is 30°C.

[0046] Weigh various impurity reference substances, add mobile phase to dissolve and dilute to prepare about 100μg / ml each impurity stock solution.

[0047] Hydroquinone and p-benzoquinone reference substance solution: Measure each appropriate amount of hydroquinone and p-benzoquinone stock solution, and dilute with mobile phase to prepare a reference substance containing both hydroquinone and p-benzoquinone about 1μg / ml Solution.

[0048] Impurity J reference solution: Measure an appropriate amount of impurity J stock solution and dilute with mobile phase to prepare a reference solution of about 1μg / ml...

Embodiment 2

[0056] Using a phenyl-bonded silica gel column, the mobile phase is the aqueous phase (2.72g potassium dihydrogen phosphate and 1.73g sodium octane sulfonate, dissolved in 872ml water, add phosphoric acid to adjust the pH to 2.15)-methanol-tetrahydrofuran (872:110 :18), the flow rate is 1.2ml / min, the detection wavelength is 220nm, and the column temperature is 30°C.

[0057] Weigh various impurity reference substances, add mobile phase to dissolve and dilute to prepare about 100μg / ml of each impurity stock solution.

[0058] Mesalazine solution containing impurities A, B, C, D, F, O, P, and hydroquinone: Weigh an appropriate amount of mesalazine, and add impurities A, B, C, D, F, O, P, An appropriate amount of benzenediol stock solution, add mobile phase to dissolve and dilute to make containing mesalazine about 2mg / ml, containing impurities A and C about 0.2μg / ml, containing impurities B, D, F, O, P, p-benzene Diphenols are about 1μg / ml solution, which is obtained.

[0059] Impur...

Embodiment 3

[0067] Using a phenyl-bonded silica gel column, the mobile phase is the aqueous phase (4.43g potassium dihydrogen phosphate and 1.63g sodium octane sulfonate, dissolved in 870ml of water, add phosphoric acid to adjust the pH to 2.15)-methanol-acetonitrile-tetrahydrofuran (870 :108:4:18), the flow rate is 1.2ml / min, the detection wavelength is 220nm, and the column temperature is 25°C.

[0068] Weigh various impurity reference substances, add mobile phase to dissolve and dilute to prepare about 100μg / ml of each impurity stock solution.

[0069] Mesalazine solution containing impurities A, B, C, D, F, O, P, and hydroquinone: Weigh an appropriate amount of mesalamine, add impurities A, B, C, D, F, O, P, An appropriate amount of benzenediol stock solution, add mobile phase to dissolve and dilute to make containing mesalazine about 2mg / ml, containing impurities A and C about 0.2μg / ml, containing impurities B, D, F, O, P, p-benzene Diphenols are about 1μg / ml solution, which is obtained....

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Abstract

The invention relates to a method for detecting specific impurities of mesalazine, belonging to the technical field of medicines. According to the invention, a phenyl bonded silica gel is used as a monomer for a chromatographic column, a mobile phase is prepared by mixing an organic phase with a buffer salt solution containing an ion-pairing agent according to a certain ratio, and elution is carried out. The method of the invention can simultaneously detect a plurality of specific impurities of mesalazine, has good specificity, high detection sensitivity and good precision, and is applicable to detection of specific impurities of mesalazine bulk drugs and to specificity of detection of specific impurities of delayed-release mesalazine tablets.

Description

Technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for detecting related substances of raw materials and pharmaceutical preparations, and in particular to a method for detecting specific impurities of mesalazine, a therapeutic drug for ulcerative colitis. Background technique [0002] Mesalazine is a drug used to treat ulcerative colitis and Crohn's disease. Most of the common preparations of the drug are absorbed by the small intestine after oral administration, so that the amount of the drug reaching the lesions of the colon is reduced and the efficacy is lost. The efficacy of mesalazine depends on its effect on the surface of the intestinal wall. Because it is acid-prone when taken orally, it is rapidly absorbed in the proximal small intestine, metabolized in the liver or small intestinal mucosa, and excreted through the kidneys, about 90% of the intake It exists in the urine in the form of acetylation, but does not reach ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 王杏林尹东东杨志强张坤
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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