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High performance liquid chromatography analysis method for avanafil and preparation thereof

A technology of high-performance liquid chromatography and avanafil, which is applied in the field of drug analysis, can solve the problems of no literature reports on the analysis methods of raw materials and their preparations, and achieve the effects of good applicability, high feasibility, and good stability

Inactive Publication Date: 2016-12-07
南京从一医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, avanafil and its preparations have not been marketed in China, and there is no literature report on the analysis method of the raw material drug and its preparations.

Method used

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  • High performance liquid chromatography analysis method for avanafil and preparation thereof
  • High performance liquid chromatography analysis method for avanafil and preparation thereof
  • High performance liquid chromatography analysis method for avanafil and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Avanafil Raw Material Related Substance Inspection

[0039] Instrument and chromatographic conditions:

[0040] Chromatographic column: Agilent C 18; 4.6mmX 150mm, 3.5um

[0041] Mobile phase: acetonitrile: 50mmol / L phosphate buffer = 40:60

[0042] Detection wavelength: 220nm

[0043] Flow rate: 1.0ml / min

[0044] Column temperature: 40°C

[0045] Injection volume: 20uL

[0046] High performance liquid chromatography: Shimadzu LC-20A, PDA detector

[0047] Experimental steps:

[0048] Solution preparation:

[0049] Get an appropriate amount of avanafil raw material drug, accurately weighed, add mobile phase to dissolve and dilute to make a solution containing about 0.5-1mg in every 1ml, and check the test solution as related substances; accurately measure 1ml of the test solution, Put in a 100ml measuring bottle, add mobile phase and dilute to the mark, shake well, and use as reference substance solution; precision measures need testing solution and reference s...

Embodiment 2

[0058] Determination of avanafil raw material content

[0059] Instrument and Chromatographic Conditions

[0060] Chromatographic column: Agilent C 18; 4.6mmX 150mm, 3.5um

[0061] Mobile phase: acetonitrile: 50mmol / L phosphate buffer = 60:40

[0062] Detection wavelength: 220nm

[0063] Flow rate: 1.0mL / min

[0064] Column temperature: 40°C

[0065] Injection volume: 20ul

[0066] Instrument: Japan Shimadzu LC-20A (PDA detector)

[0067] Solution preparation

[0068]Accurately weigh 10 mg of avanafil self-made raw material, put it in a 100ml volumetric flask, add an appropriate amount of mobile phase, shake to dissolve and dilute to the scale, shake well, and obtain the mother liquor of the test sample; accurately measure the mother liquor of the test sample 1ml, put In a 10ml measuring bottle, add mobile phase to dilute to the mark, shake well, and as a reference solution, accurately measure 20ul and inject it into a liquid chromatograph, and record the chromatogram; ...

Embodiment 3

[0076] Avanafil Tablet Related Substance Inspection

[0077] Instrument and chromatographic conditions:

[0078] Chromatographic column: Agilent C 18; 4.6mmX 150mm, 3.5um

[0079] Mobile phase: acetonitrile: 50mmol / L phosphate buffer = 40:60

[0080] Detection wavelength: 220nm

[0081] Flow rate: 1.0ml / min

[0082] Column temperature: 40°C

[0083] Injection volume: 20ul

[0084] Instrument: Japan Shimadzu LC-20A (PDA detector)

[0085] Solution preparation:

[0086] Take avanafil tablet, grind it to powder, take an appropriate amount of the ground powder, accurately weigh it, add mobile phase to dissolve and dilute it to make a solution containing about 0.5-1mg per 1ml, filter and take the subsequent filtrate as the relevant Substance inspection need testing solution; precision measures need testing solution 1ml, puts in 100ml measuring bottle, adds mobile phase and dilutes to scale, shakes up, as reference solution; precision measures need testing solution and each 2...

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Abstract

The present invention provides a high performance liquid chromatography analysis method for avanafil and a preparation thereof, and belongs to the technical field of drug analysis. According to the high performance liquid chromatography analysis method, a chromatographic column selecting an octadecyl-bonded silica gel as a filler is selected, the specification is 4.6 mm*150 mm, 5 [mu]m, 4.6 mm*200 mm, 5 [mu]m, 4.6 mm*250 mm, 5 [mu]m, 4.6 mm*150 mm, 3.5 [mu]m, 4.6 mm*200 mm, 3.5 [mu]m, 4.6 mm*250 mm, 3.5 [mu]m, the mobile phase is an acetonitrile-buffer salt according to a ratio of 30-70:70-30, the flow rate is 5-1.5 ml / min, the column temperature is 30-40 DEG C, the wavelength of an ultraviolet detector is 200-300 nm, and the injection volume is 5-50 [mu]l. According to the present invention, the method only uses the ordinary liquid chromatograph, the requirement on the equipment is not high, the two mediums selected by the mobile phase are generally easy to obtain, the feasibility is high, the operation process is simple and convenient, the applicability is good, and the method can be widely used in avanafil and the preparation thereof.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high performance liquid chromatography analysis method of avanafil and its preparation. Background technique [0002] Avanafil (Avanafil), the chemical name is 4-[(3-chloro-4-methoxybenzyl)amino]-2-[2-(hydroxymethyl)-1-pyrrolidinyl]-N- (2-Pyrimidinylmethyl)-5-pyrimidinemethanesulfonamide, CAS Accession No. 330784-47-9. The chemical structural formula is as follows: [0003] [0004] Avanafil is a phosphodiesterase 5 (PDE5) inhibitor, a research project transferred by Vivus from Mitsubishi Tanabe Pharmaceutical Company of Japan. For the treatment of male erectile dysfunction (ED), launched on April 27, 2012, in the form of tablets (50mg, 100mg and 200mg) [0005] Avanafil is a PDE5 inhibitor that can effectively inhibit the degradation of cGMP in the penis, increase the level of cGMP in the penis, cause the smooth muscle of the corpus cavernosum to relax ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 陈维生黄明辉黄玉晔施润杰吴锦慧
Owner 南京从一医药科技有限公司
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