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Content determination of tofacitinib citrate and detection method of related substances

A technology of tofacitinib and citric acid, which is applied in the field of drug analysis, can solve the problems such as the content of raw materials and the analysis method of related substances that are not reported in literature, and achieve good repeatability and recovery rate, accurate content determination results, and detection. high rate effect

Active Publication Date: 2016-03-09
NANJING CORE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the dosage form of tofacitinib citrate that has been marketed is a tablet with a specification of 5 mg. However, due to data protection and other reasons, there are no literature reports on the content of this raw material and the analysis method of related substances.

Method used

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  • Content determination of tofacitinib citrate and detection method of related substances
  • Content determination of tofacitinib citrate and detection method of related substances
  • Content determination of tofacitinib citrate and detection method of related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Determination of reversed-phase high-performance liquid chromatography of tofacitinib citrate content

[0020] Chromatographic conditions and system suitability test take octadecyl silane bond and silica gel as filler; with acetonitrile-0.05mol / L ammonium acetate (90:10) as mobile phase A, with acetonitrile-0.05mol / L ammonium acetate (10 :90) is mobile phase B; Carry out gradient elution according to the following table. The flow rate is 1.0ml per minute; the detection wavelength is 286nm. The number of theoretical plates is not less than 4000 based on the peak of tofacitinib.

[0021]

[0022] The following items of the assay method were verified:

[0023] 1. Linearity and range

[0024] Take about 10mg of tofacitinib citrate reference substance, accurately weigh it, put it in a 50ml measuring bottle, add mobile phase to ultrasonically dissolve and dilute to the mark; accurately measure 1.0, 1.5, 2.0, 2.5, 3.0ml to a 10ml measuring bottle In the solut...

Embodiment 2

[0048] Embodiment 2: Determination of related substances of tofacitinib citrate by reversed-phase high-performance liquid chromatography

[0049] Determine according to high performance liquid chromatography (Chinese Pharmacopoeia 2010 edition two appendix VD).

[0050] Chromatographic conditions and system suitability test use octadecylsilane bond and silica gel as filler; use acetonitrile-50mmol / L ammonium acetate (9:1) as mobile phase A; use acetonitrile-50mmol / L ammonium acetate (1:9 ) is the mobile phase B to carry out linear gradient elution according to the table. The flow rate is 1.0ml per minute; the detection wavelength is 286nm. Take tofacitinib citrate known impurity Ⅰ (intermediate 3), impurity Ⅱ (intermediate 2), impurity Ⅲ (starting material 2), impurity Ⅳ (intermediate 1), isomers (not enantiomer) and appropriate amount of tofacitinib citrate, add acetonitrile to ultrasonically dissolve and dilute to make each 1ml containing known impurity Ⅰ (intermediate 3), i...

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Abstract

The invention discloses a content determining and related substance detection method for tofacitinib citrate. The method is mainly used for determining and examining medicinal raw materials of tofacitinib citrate and related substances by using efficient liquid chromatography. The method disclosed by the invention is high in detection rate of the related substances, high in precision, accurate in content determining result and good in repeatability and recovery rate. The method verified can be used for routine analysis and quality control of raw materials of tofacitinib citrate and a preparation sample.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular, relates to a quality control method of tofacitinib citrate crude drug, in particular to a method for determining the content of tofacitinib citrate and detecting related substances. Background technique [0002] Tofacitinib citrate, English name Tofacitinibcitrate, this product is 3-((3R,4R)-4-methyl-3-(methyl-7H-pyrrolo[2,3-d]pyrimidine-4- Amino)-β-oxo-1-piperidine propionitrile, 2-hydroxy-1,2,3-propane tricarboxylate (1:1). Tofacitinib citrate is produced by Japan Takeda Pharmaceutical Co., Ltd. Co., Ltd. and Pfizer of the United States jointly developed a new drug for adult patients with moderately to severely active rheumatoid arthritis (RA) who have insufficient response or intolerance to methotrexate treatment. It was approved by the US FDA on November 6, 2012 listed under the trade name [0003] Rheumatoid arthritis (AA) is a chronic systemic autoimmune disease cha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
Inventor 王雪根何凌云王园园田春梅汪洋
Owner NANJING CORE TECH CO LTD