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A method and application of high performance liquid chromatography for detecting related substances of camostat mesylate

A technology of camostat mesilate and high performance liquid chromatography, which is applied in the field of medicine, can solve problems such as poor stability and complex impurity spectrum of camostat mesilate, and achieve low sensitivity, increased retention time, and high detection The effect of sensitivity

Active Publication Date: 2022-04-26
天津泰普制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Camostat mesylate has extremely complex impurity profile, poor stability and easy degradation

Method used

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  • A method and application of high performance liquid chromatography for detecting related substances of camostat mesylate
  • A method and application of high performance liquid chromatography for detecting related substances of camostat mesylate
  • A method and application of high performance liquid chromatography for detecting related substances of camostat mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1) Experimental conditions

[0048] Agilent1260-DAD high performance liquid chromatograph;

[0049] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0050] Flow rate: 1.0mL / min;

[0051] Column temperature: 35°C;

[0052] Injection volume: 10 μL;

[0053] Sample concentration: 1mg / ml;

[0054] Diluent: 90% acetonitrile aqueous solution;

[0055] Detection wavelength: 230nm and 265nm;

[0056]Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.1% (volume fraction) of trifluoroacetic acid.

[0057] Mobile Phase B: Acetonitrile

[0058]

[0059] 2) Solution preparation

[0060] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent and dilute quantitatively Make a solution containi...

Embodiment 2

[0069] Experimental conditions:

[0070] Agilent1260-DAD high performance liquid chromatograph;

[0071] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0072] Flow rate: 1.0mL / min;

[0073] Detection wavelength: 230nm and 265nm;

[0074] Column temperature: 35°C;

[0075] Injection volume: 10 μL;

[0076] Sample concentration: 1mg / ml;

[0077] Diluent: 90% acetonitrile aqueous solution;

[0078] Detection wavelength: 230nm and 265nm;

[0079] Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.05% (volume fraction) of trifluoroacetic acid.

[0080] Mobile Phase B: Acetonitrile

[0081]

[0082] 2) Solution preparation

[0083] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent an...

Embodiment 3

[0092] Experimental conditions:

[0093] Agilent1260-DAD high performance liquid chromatograph;

[0094] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0095] Flow rate: 0.8mL / min;

[0096] Detection wavelength: 230nm and 265nm;

[0097] Column temperature: 35°C;

[0098] Injection volume: 10 μL;

[0099] Sample concentration: 1mg / ml;

[0100] Diluent: 90% acetonitrile aqueous solution;

[0101] Detection wavelength: 230nm and 265nm;

[0102] Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.10% (volume fraction) of trifluoroacetic acid.

[0103] Mobile Phase B: Acetonitrile

[0104]

[0105] 2) Solution preparation

[0106] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent an...

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Abstract

The invention provides a method for detecting related substances of camostat mesylate by using high performance liquid chromatography, wherein the chromatographic column is an octadecylsilane bonded silica gel chromatographic column, and the mobile phase A is sodium heptanesulfonate and three A mixed solution of fluoroacetic acid; the mobile phase B is acetonitrile, methanol, ethanol, tetrahydrofuran or a mixture of both; the diluent is pure water or a mixture of methanol, acetonitrile, ethanol, or tetrahydrofuran solution; this method can be used for the determination of related substances of camostat mesylate and the determination of the residual amount in the medicine using 4-dimethylaminopyridine as catalyst and N,N-dimethylformamide as refining solvent in the synthesis process Determination of applications.

Description

technical field [0001] The invention belongs to the technical field of medicine, and specifically provides a method for detecting related substances of camostat mesylate by using high-performance liquid chromatography, and the detection method adopts liquid chromatography. Background technique [0002] Camostat mesilate (English name: Camostat Mesilate) chemical name becomes 2-(dimethylamino)-2-oxoethyl 4-(4-guanidinobenzoyloxy)phenylacetate A Sulfonate, molecular formula C 20 h 22 N 4 o 5 •CH 3 SO 3 H, molecular weight 494.52, CAS accession number: 59721-29-8. Its structure is as shown in formula I: [0003] [0004] Camostat mesylate is a non-peptide protein inhibitor. After oral administration, camostat mesylate quickly acts on the body's kinin production system, fibrinolytic system, coagulation system and complement system, inhibiting the abnormal hyperactivity of enzyme activities in these systems, thereby controlling the symptoms of chronic pancreatitis and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74G01N30/06G01N30/04G01N30/88
CPCG01N30/02G01N30/34G01N30/74G01N30/06G01N30/04G01N30/88G01N2030/047G01N2030/884G01N2030/8872
Inventor 张慕军石涛雷勇胜邓瑶崔轶达丁文宇刘桂霞史可吟
Owner 天津泰普制药有限公司