Method for detecting related substances in Loxoprofen or sodium salt thereof

A detection method and related substance technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that the purpose of detection cannot be achieved, and whether it cannot be detected effectively, and achieve good peak shape, large income, and simple reagents Effect

Active Publication Date: 2019-09-20
HUNAN JIUDIAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] After repeated experiments and verification, under this method, the peak shape of the impurity DP-3 is tailed, and it is impossible to effectively detect whether there is such an impurity as DP-3, and the purpose of detection cannot be achieved.
[0014] Therefore, under the condition that the DP-3 impurity in loxoprofen or its sodium salt

Method used

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  • Method for detecting related substances in Loxoprofen or sodium salt thereof
  • Method for detecting related substances in Loxoprofen or sodium salt thereof
  • Method for detecting related substances in Loxoprofen or sodium salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Take 1 loxoprofen sodium gel patch, cut the middle part 35cm 2 (equivalent to 25mg of loxoprofen sodium), cut into pieces into a 150ml conical flask, add 50ml of methanol, accurately weigh, sonicate for 30 minutes, let cool, add methanol to make up for the lost weight, filter, and take the subsequent filtrate , that is, the test solution is obtained. Precisely measure 10 μl of the test solution, inject it into a liquid chromatograph, measure and record the chromatogram.

[0066] The chromatographic conditions are as follows:

[0067] Column: Agilent Eclipse XDB-C18 4.6×150mm; 5μm

[0068] Mobile phase: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2.5 and methanol gradient elution; detection wavelength: 222nm; flow rate: 1.0ml / min; column temperature: 35℃

[0069] The gradient elution procedure is as follows:

[0070] A: methanol;

[0071] B: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2....

Embodiment 2

[0075] Take 1 loxoprofen sodium gel patch, cut the middle part 35cm 2 (equivalent to 25mg of loxoprofen sodium), cut into pieces into a 150ml conical flask, add 50ml of methanol, accurately weigh, sonicate for 30 minutes, let cool, add methanol to make up for the lost weight, filter, and take the subsequent filtrate , that is, the test solution is obtained. Precisely measure 10 μl of the test solution, inject it into a liquid chromatograph, measure and record the chromatogram.

[0076] The chromatographic conditions are as follows:

[0077] Column: Agilent Eclipse XDB-C18 4.6×150mm; 5μm

[0078] Mobile phase: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2.5 and methanol gradient elution; detection wavelength: 222nm; flow rate: 1.0ml / min; column temperature: 35℃

[0079] The gradient elution procedure is as follows:

[0080] A: methanol;

[0081] B: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2....

Embodiment 3

[0085] Take 1 loxoprofen sodium gel patch, cut the middle part 35cm 2 (equivalent to 25mg of loxoprofen sodium), cut into pieces into a 150ml conical flask, add 50ml of methanol, accurately weigh, sonicate for 30 minutes, let cool, add methanol to make up for the lost weight, filter, and take the subsequent filtrate , that is, the test solution is obtained. Precisely measure 10 μl of the test solution, inject it into a liquid chromatograph, measure and record the chromatogram.

[0086] The chromatographic conditions are as follows:

[0087] Column: Agilent Eclipse XDB-C18 4.6×150mm; 5μm

[0088] Mobile phase: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2.5 and methanol gradient elution; detection wavelength: 222nm; flow rate: 1.0ml / min; column temperature: 35℃

[0089] The gradient elution procedure is as follows:

[0090] A: methanol;

[0091] B: 0.01mol / L sodium dihydrogen phosphate solution, add phosphoric acid to adjust pH to 2....

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Abstract

The invention discloses a method for detecting related substances in Loxoprofen or sodium salt thereof. The method uses a high performance liquid chromatography, gives unique chromatographic conditions and successfully detects a process impurity in the Loxoprofen sodium salt. According to the method, the impurities in the process are detected by using a reverse chromatography, the peak shape is better, the separation degree between the peak shape and an adjacent chromatographic peak is high, the research and development cost is saved, the experiment difficulty is reduced, and the reproducibility is good.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting related substances in loxoprofen or its sodium salt. Background technique [0002] Loxoprofen Sodium (Loxoprofen Sodium), the chemical name is 2-[4-(2-oxocyclopentane-1-ylmethyl)phenyl]sodium propionate dihydrate, CAS number: 80382-23- 6. The molecular formula is C 15 h 17 NaO 3 , the molecular weight is 268.28, and the structural formula is as follows: [0003] [0004] Loxoprofen sodium was first developed by Japan's Daiichi Sankyo Co., Ltd., and this product has been included in the National Ninth Five-Year Plan and one of the recommended trial products for new product development in 2010. Loxoprofen sodium is an acrylic acid precursor non-steroidal anti-inflammatory drug, which itself has no pharmaceutical activity. After transdermal or oral administration and absorption, it will be converted into the active metabolite trans-OH body in the ...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N30/34G01N30/28G01N30/74G01N30/06G01N30/14
CPCG01N30/06G01N30/14G01N30/28G01N30/34G01N30/74G01N30/89
Inventor 文凤何莉谢超君殷报云王奕彭靖
Owner HUNAN JIUDIAN PHARMA
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