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Method for detecting sildenafil citrate impurities

A technology for the detection of sildenafil citrate and its detection method, which is applied in the detection field of sildenafil citrate impurities, can solve the problems of large consumption of organic solvents, failure to obtain effective separation, incomplete separation of impurities, etc., and achieve Saving organic solvents, shortening detection time, and high sensitivity

Active Publication Date: 2021-01-08
GUANGZHOU BAIYUNSHAN PHARMA HLDG CO LTD BAIYUNSHAN PHARMA GENERAL FACTORY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] CN105334275A discloses a method for detecting related substances of sildenafil citrate. The method adopts high performance liquid chromatography, uses octadecylsilane bonded silica gel as the chromatographic column of the stationary phase, and ammonium acetate aqueous solution as the mobile phase A , acetonitrile-methanol is mobile phase B, detection wavelength is 292nm, gradient elution, although can separate and detect 7 kinds of related substances in sildenafil citrate at the same time, but in these 7 kinds of related substances only impurities D, E, G corresponds to the impurities D, B, and A recorded in EP9.2, and the remaining EP9.2 impurities C, E, F, and G cannot be effectively separated, and the separation takes more than 20 minutes
[0015] In summary, it can be seen that the existing detection methods for related substances of sildenafil citrate have shortcomings such as few impurities that can be separated, some impurities are not completely separated, and the time is long and the consumption of organic solvents is large.

Method used

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  • Method for detecting sildenafil citrate impurities
  • Method for detecting sildenafil citrate impurities
  • Method for detecting sildenafil citrate impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Mix sildenafil citrate and 7 kinds of sildenafil citrate EP impurities to obtain the sample to be tested, prepare the test solution by conventional methods in this field, and use the following different chromatographic conditions for detection.

[0041] method one:

[0042] Instrument: Waters Acquity UPLC system

[0043] Chromatographic column: Waters Acquity UPLC BEH C18 chromatographic column (100mm×2.1mm, 1.7μm)

[0044] Mobile phase A: Phosphate buffer (pH 5.5, preparation method: take 2.72g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, adjust the pH to 5.5 with 120g / L potassium hydroxide aqueous solution)-acetonitrile (80:20, v / v )

[0045] Mobile phase B: Phosphate buffer (pH 5.5)-methanol-acetonitrile (20:25:55, v / v / v)

[0046] Flow rate: 0.5ml / min

[0047] Injection volume: 4μl

[0048] Detection wavelength: 240nm

[0049] Column temperature: 25°C

[0050] Elution procedure: 0~1min, mobile phase A: mobile phase B volume ratio is 75:2...

Embodiment 2

[0101] The chromatographic conditions of Method 1 in Example 1 are used below to study the adaptability, specificity, limit of quantification, limit of detection, repeatability, etc. of the detection method of the present invention.

[0102] Solution preparation:

[0103] Need testing solution: get an appropriate amount of sildenafil citrate oral preparations to be tested (approximately containing sildenafil 50mg), accurately weighed, put in a 100ml measuring bottle, add an appropriate amount of mobile phase A, ultrasonically dissolve, put After cooling, adjust the volume to the mark, shake well, and filter.

[0104] Reference substance solution: take an appropriate amount of sildenafil citrate reference substance (National Inspection Institute, batch number 420012-201702, converted after desalination), accurately weighed, add mobile phase A to dissolve and quantitatively dilute to make about A solution of 1 μg of sildenafil.

[0105] According to the chromatographic conditi...

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Abstract

The invention discloses a method for detecting sildenafil citrate impurities, which adopts UPLC (Ultra Performance Liquid Chromatography) for detection, takes a buffer solution-methanol- acetonitrileas as a mobile phase, and the pH value of the buffer solution is 5.5-6.8. According to the method, the sildenafil citrate impurities are detected by adopting the UPLC, the sildenafil citrate impurities can be quickly eluted and separated by adopting the mobile phase with specific composition, the detection time is shortened, and seven sildenafil citrate EP impurities can be separated by further adjusting the composition of the mobile phase and chromatographic conditions.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a method for detecting impurities of sildenafil citrate. Background technique [0002] Sildenafil Citrate Tablets is a selective inhibitor of cyclic guanosine monophosphate (cGMP)-specific phosphodiesterase type 5 (PDE5), originally developed by Pfizer, USA, with the trade name Viagra, and the dosage form is tablets. The specifications are 0.1g, 50mg and 25mg, and the indication is erectile dysfunction. Viagra was first launched in Italy on April 1, 1998, and is an oral drug for the treatment of erectile dysfunction. Sildenafil is suitable for different indications according to different specifications, (or) dosage forms, usage and dosage. At present, it can also be used clinically for the treatment of pulmonary arterial hypertension. The dosage form is: tablet (20mg specification), orally disintegrating film (20mg specification) and multi-dose dry suspension (900mg specification)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/34G01N30/86
CPCG01N30/02G01N30/14G01N30/34G01N30/8634
Inventor 王玮李翠芬罗志波王健松
Owner GUANGZHOU BAIYUNSHAN PHARMA HLDG CO LTD BAIYUNSHAN PHARMA GENERAL FACTORY
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