Detection method for sildenafil citrate related substances

A technology of sildenafil citrate and related substances, applied in the field of drug analysis, can solve problems such as poor separation, inability to detect at the same time, difficulty in quality control of sildenafil citrate raw materials and its preparations, etc. , to achieve the effect of high resolution and simple method

Active Publication Date: 2016-02-17
CHANGZHOU YABANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When this method is used to analyze and detect the 7 related substances A to G in the above table, the related substance D is not detected, the separation degree of the related substances A and E is not good, and the number of theoretical plates is low
[0014] In summary, none of the existing methods can simultaneously detect the 7 related substances of sildenafil citrate in the above table, and the mobile phase in the chromatographic conditions contains non-volatile salts or triethylamine, which cannot be used for liquid mass spectrometry Joint analysis, affecting the development of follow-up research work
[0015] In view of the inability of existing technologies and methods to simultaneously detect the 7 related substances of sildenafil citrate in the above table, it brings difficulties to the quality control of sildenafil citrate API and its preparations

Method used

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  • Detection method for sildenafil citrate related substances
  • Detection method for sildenafil citrate related substances
  • Detection method for sildenafil citrate related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1: Prepare system suitability solution:

[0037] Take related substances A, B, C, D, E, F, G and sildenafil citrate reference substance, weigh them accurately, add mobile phase to prepare a mixed control solution, and the concentration of related substances A to G is 5 μg / ml, the concentration of sildenafil citrate is 200μg / ml.

[0038] Step 2: Carry out the determination of related substances according to the following high performance liquid chromatography conditions:

[0039] Use octadecylsilane bonded silica gel as the filler, ammonium acetate containing 5mmol / ml, adjust the pH to 7.0 with ammonia water as the mobile phase A, use acetonitrile:methanol=1:1 as the mobile phase B, and the column temperature 30°C, the flow rate is 1ml / min, the detection wavelength is 292nm, gradient elution is carried out by HPLC, and the mobile phase gradient is as follows:

[0040]

[0041] The theoretical plate number of the main component is 73453, and the resolution betwee...

Embodiment 2

[0044] Step 1: Prepare system suitability solution:

[0045] Take related substances A, B, C, D, E, F, G and sildenafil citrate reference substance, weigh them accurately, add mobile phase to prepare a mixed control solution, and the concentration of related substances A to G is 5 μg / ml, the concentration of sildenafil citrate is 200μg / ml.

[0046] Step 2: Carry out the determination of related substances according to the following high performance liquid chromatography conditions:

[0047] Use octadecylsilane bonded silica gel as the filler, use ammonium acetate containing 6mmol / ml, adjust the pH to 7.0 with ammonia water as the mobile phase A, use acetonitrile:methanol=1:1 as the mobile phase B, and the column temperature 30°C, the flow rate is 1ml / min, the detection wavelength is 292nm, gradient elution is carried out by HPLC, and the mobile phase gradient is as follows:

[0048]

[0049] The theoretical plate number of the main component is 89369, and the resolution ...

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Abstract

The invention discloses a detection method for sildenafil citrate related substances. The high performance liquid chromatography is adopted in the detection method, octadecylsilane bonded silica gel is used as a chromatographic column for the stationary phase, an ammonium acetate water solution is used as the mobile phase A, an acetonitrile-methyl alcohol mixture is used as the mobile phase B, the detection wavelength is 292 nm, and gradient elution is carried out. The detection method is simple, efficient, high in resolution and capable of separating and detecting seven related substances in sildenafil citrate at the same time, and the mobile phases are suitable for mass spectrometric detection and can be used for quality research and quality control over sildenafil citrate raw material drugs and preparation products.

Description

technical field [0001] The invention relates to a chemical drug sildenafil citrate and a method for detecting related substances of its preparation, belonging to the field of drug analysis. Background technique [0002] Sildenafil citrate is an effective drug for the treatment of erectile dysfunction caused by subjective and objective reasons. It is a selective phosphodiesterase type 5 (PDE-5) inhibitor, approved by FDA in March 1997 Available as a prescription drug in the United States. The chemical structural formula of sildenafil citrate is as follows: [0003] [0004] The main cause of penile erectile dysfunction is insufficient blood supply to the cavernous body of the penis, which may be related to the lack of nitric oxide. NO can activate guanylate cyclase (GC), under the action of activated GC, guanylate (GTP) is converted into cyclic guanylate (cGMP); cGMP can be phosphodiesterase type 5 (PDE-5 ) is degraded to cGMP-5', which has no biological effect, while c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 陈再新王璠王勇军黄静周慧琴
Owner CHANGZHOU YABANG PHARMA
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