Determination method of p-toluenesulfonate esters in racecadotril

A technology of p-toluenesulfonate and racecadotril, which is applied in the field of medicine, can solve the problems of expensive GC-MS instruments, low penetration rate, complicated operation, etc., and achieve improved drug safety, good separation effect, exclusive strong effect

Active Publication Date: 2021-07-02
SHANDONG BOYUAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to overcome the deficiencies such as expensive GC-MS instrument, popularization rate is not high, complicated operation, etc., provides a kind of HPLC method that is simpler and easier to simultaneously detect three kinds of p-toluenesulfonic acid esters

Method used

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  • Determination method of p-toluenesulfonate esters in racecadotril
  • Determination method of p-toluenesulfonate esters in racecadotril
  • Determination method of p-toluenesulfonate esters in racecadotril

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1 Instruments and materials

[0044] 1.1 Instrument: Waters e2695 high performance liquid chromatography.

[0045] 1.2 Reagents: acetonitrile (chromatographic grade), potassium dihydrogen phosphate, phosphoric acid (reagent grade), and pure water.

[0046] 2 Methods and results

[0047] 2.1 Chromatographic conditions

[0048] Chromatographic column: Germany Merck LiChrospher RP 18 (end-capped, 250mm×4.0mm×5μm);

[0049] Mobile phase A: put 1.0g potassium dihydrogen phosphate in 1000ml water, adjust the pH to 2.5 with phosphoric acid;

[0050] Mobile phase B: acetonitrile;

[0051] Solvent: acetonitrile;

[0052] Detector: UV detector;

[0053] Detection wavelength: 225nm;

[0054] Flow rate: 1.0ml / min;

[0055] Column temperature: 40°C;

[0056] Injection volume: 10μl;

[0057] See Table 2 for gradient elution conditions.

[0058] Table 2 Gradient elution table

[0059] time (minutes) Mobile phase A(%) Mobile phase B(%) 0 60 40 5 60 ...

Embodiment 2

[0107] Embodiment 2: the detection of actual sample

[0108] 1) cancel the carcadotril bulk drug, dissolve with acetonitrile, be mixed with the solution that contains 20mg racecadotril in 1ml, as need testing solution;

[0109] 2) Dissolve the methyl p-toluenesulfonate reference substance, ethyl p-toluenesulfonate reference substance and isopropyl p-toluenesulfonate reference substance with acetonitrile, and prepare 1ml containing 0.1 μg methyl p-toluenesulfonate reference substance, A solution of 0.1 μg ethyl p-toluenesulfonate reference substance and 0.1 μg isopropyl p-toluenesulfonate reference substance;

[0110] 3) Get the need testing solution prepared in step 1) and the reference solution in step 2), adopt the same instruments and reagents as in Example 1, and detect according to the chromatographic conditions shown in step 1) 2.1.

[0111] 4) According to the external standard method, calculate the content of methyl p-toluenesulfonate, ethyl p-toluenesulfonate and iso...

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Abstract

The invention discloses a detection method for p-toluenesulfonate substances in racecadotril. The method uses German Merck LiChrospher RP 18 as a chromatographic column, and adopts HPLC detection method to carry out qualitative and quantitative analysis of methyl p-toluenesulfonate, ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in racecadotril analyze. The method has been validated in the present invention, and experiments prove that the method has the advantages of strong specificity, rapidity, sensitivity, accuracy and the like. The present invention establishes the qualitative and quantitative methods for the genotoxic impurities methyl p-toluenesulfonate, ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate in racecadotril for the first time, which facilitates the quality control of racecadotril Controlling, thereby improving the drug safety of racecadotril.

Description

technical field [0001] The invention relates to a detection method for genotoxic impurities in racecadotril, in particular to p-toluenesulfonate esters (methyl p-toluenesulfonate, ethyl p-toluenesulfonate and isopropyl p-toluenesulfonate) The HPLC detection method belongs to the technical field of medicine. Background technique [0002] Racecadotril is a neprilysin inhibitor developed by the French company Bioprojet, and was launched in France in 1993 under the trade name Tiorfan. As an antidiarrheal drug with a new mechanism of action, racecadotril can directly inhibit excessive intestinal secretion and rapidly improve diarrhea symptoms. Acute diarrhea in adults and infants and children older than 1 month. Soon after it was launched, the Canadian Pediatric Association and the U.S. Centers for Disease Control and Prevention listed racecadotril as an essential drug for the treatment of children with diarrhea. In 2011, it was also included in the recommended drug of the Chin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/36
CPCG01N30/02G01N30/36G01N2030/047
Inventor 刘旭晶孙庆伟邹秀婷王先菊杜方鹏
Owner SHANDONG BOYUAN PHARM CO LTD
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