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Method for detecting trinitride compounds in candesartan cilexetil

A technology of candesartan cilexetil and azide compounds, which is applied in the field of detection of azide compounds in candesartan cilexetil, can solve the problems of time-consuming and cumbersome steps

Active Publication Date: 2019-11-29
HINYE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method requires derivatization operations, which are cumbersome and time-consuming

Method used

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  • Method for detecting trinitride compounds in candesartan cilexetil
  • Method for detecting trinitride compounds in candesartan cilexetil
  • Method for detecting trinitride compounds in candesartan cilexetil

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Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: the HPLC detection of candesartan cilexetil bulk drug

[0032] Adopt detection method of the present invention, specific implementation is as follows:

[0033] Instrument: Waters e2695-2489 high performance liquid chromatography

[0034] Chromatographic column: Octadecylsilane bonded silica gel as filler (Waters Atlantis T3 C18 4.6*250mm, 5μm)

[0035] Mobile phase A: The volume ratio of acetonitrile and sulfuric acid aqueous solution is 40:60 as mobile phase A.

[0036] Mobile phase B: The volume ratio of acetonitrile to water is 90:10 as mobile phase B.

[0037] Carry out gradient elution according to the following table 1:

[0038] Table 1 Elution program

[0039]

[0040] Column temperature: 30°C

[0041] Flow rate: 0.7ml / min

[0042] Injection volume: 50μl

[0043] Detection wavelength: 205nm

[0044] Workstation: Empower 3

[0045] Test solution: Accurately weigh about 80 mg of candesartan cilexetil raw material drug to be tested, put it ...

Embodiment 2

[0050] Embodiment 2: Determination of detection wavelength

[0051] Instrument: UV-Vis spectrophotometer

[0052] Detection wavelength: 200-400nm full wavelength scanning

[0053] Accurately weigh about 30 mg of sodium azide reference substance, put it in a 250ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and use it as the reference substance mother solution. Precisely measure 5.0ml of the mother solution of the reference substance, put it in a 10ml measuring bottle, add diluent to the mark, shake well, and use it as the reference substance solution for wavelength detection.

[0054] Take an appropriate amount of sodium azide wavelength detection reference substance solution, measure according to the "UV-Vis Spectrophotometry Operating Procedures", record the spectral scanning curve, and see the attached figure 1 .

[0055] Refer to attached figure 1 , from the results of the ultraviolet scanning diagram: sodium azide has a relatively lar...

Embodiment 3

[0056]Embodiment 3: System suitability and specificity test

[0057] The system applicability of this embodiment also examines the system applicability of the instrument during continuous sample injection.

[0058] Blank solution: diluent;

[0059] Reference substance solution, system suitability solution: the preparation method is the same as in Example 1;

[0060] According to the chromatographic conditions in Example 1, 1 injection of blank solution, 6 injections of reference solution, and 1 injection of system suitability solution were sequentially injected, and the relative standard deviation of retention time and peak area was calculated, and the results are shown in Table 2.

[0061] Table 2 System Suitability Results

[0062]

[0063] Conclusion: see attached figure 2 , the blank solution has no interference. Refer to attached image 3 , in the chromatogram obtained from the reference substance solution, the signal-to-noise ratio of the azide peak is above 100...

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Abstract

The invention belongs to the technical field of chemical analysis and relates to a method for detecting trinitride compounds in candesartan cilexetil. According to the method, a to-be-tested candesartan cilexetil bulk pharmaceutical chemical product is taken, acetonitrile is added, an obtained mixture is subjected to ultrasonic dissolution, and a sulfuric acid aqueous solution is adopted to dilutean obtained solution; the volume ratio of the acetonitrile to the sulfuric acid aqueous solution ranges from 40:60 to 60:40; an obtained solution is fully shaken and then filtered, and a filtrate isadopted as a test solution for later use; and according to a chromatographic column, octadecylsilane chemically bonded silica adopted as a stationary phase, an acetonitrile-sulfuric acid aqueous solution adopted as a mobile phase A, and an acetonitrile-water solution as a mobile phase B, HPLC detection is carried out, and a spectrum is recorded. With the detection method adopted, sodium azide in the candesartan cilexetil can be quickly and conveniently separated and quantitatively measured, and therefore, the quality of a candesartan cilexetil product is effectively controlled.

Description

technical field [0001] The invention relates to the technical field of chemical drug analysis, in particular to a method for detecting azide compounds in candesartan cilexetil. [0002] technical background [0003] Candesartan cilexetil is the prodrug of candesartan, which can be rapidly and completely hydrolyzed to candesartan in the gastrointestinal tract. Candesartan is an angiotensin II AT1 receptor antagonist. It antagonizes the vasoconstriction of angiotensin II by binding to the AT1 receptor of vascular smooth muscle, thereby reducing peripheral vascular resistance. It is a long-acting receptor antagonist . [0004] Azide is one of the key intermediates in the synthesis of candesartan cilexetil, because it can inhibit the activity of cytochrome oxidase and various enzymes, and lead to abnormal phosphorylation and cellular respiration, the main acute toxicity It can cause an extreme decrease in vascular tension and is one of the common genotoxic impurities. Therefore...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34
Inventor 王洁程雪清高玉贺李力余彬彬
Owner HINYE PHARM CO LTD
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