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Method for detecting benzene and isopropylidene acetone residues in Avanafil by gas chromatography

A technology of mesityl oxide and gas chromatography, which is applied in the field of pharmaceutical analysis, can solve the problems of high toxicity and detection methods that cannot meet the detection sensitivity requirements, and achieve the effects of high separation, high sensitivity, and easy operation

Inactive Publication Date: 2019-04-30
重庆瑞泊莱医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Benzene and mesityl oxide are highly toxic. The control limit of benzene in the drug is only 2ppm, and the control limit of mesityl oxide is only 7.5ppm. Because the limit is too low, conventional detection methods cannot meet the detection sensitivity requirements, so The development and detection of the above two residual solvents in Avanafil finished products has great quality control significance

Method used

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  • Method for detecting benzene and isopropylidene acetone residues in Avanafil by gas chromatography
  • Method for detecting benzene and isopropylidene acetone residues in Avanafil by gas chromatography
  • Method for detecting benzene and isopropylidene acetone residues in Avanafil by gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Solution preparation:

[0035] Blank solvent: NMP-water (1:1) ratio mixing;

[0036] Reference solution: accurately weigh the appropriate amount of benzene and mesityl oxide, dissolve it with NMP-water (1:1) and dilute quantitatively to make a mixed control containing 0.1ug / ml of benzene and 0.375ug / ml of mesityl oxide The product solution, then accurately measure 5ml and place it in a 20ml headspace bottle, press the cap and seal, and get it;

[0037] Test solution: accurately weigh about 0.5g of the test product, place it in a 10ml measuring flask, add 5ml NMP precisely, shake it vigorously to dissolve it, then add water to dilute it to the mark and shake it well. Then precisely pipette 5ml into a 20ml headspace bottle, press the cap and seal, and it is ready;

[0038] (2) Gas chromatography detection:

[0039] The chromatographic column is Agilent DB-624 (30m*0.32mm*1.8um); the inlet temperature is 220℃; the detector temperature is 250℃; the detector is FID; the split ra...

Embodiment 2

[0045] Example 2 Method specificity test:

[0046] Accurately weigh about 0.5g of the sample to be tested, place it in a 10ml measuring flask, add 5ml of NMP precisely, shake it vigorously to dissolve it, add water to dilute it to the mark, and shake it well. Then precisely pipette 5ml into a 20ml headspace bottle, press the cap and seal, and then obtain the test solution. Accurately weigh an appropriate amount of benzene and mesityl oxide, dissolve it with NMP-water (1:1) and dilute quantitatively to make a mixed reference solution containing 0.1ug / ml of benzene and 0.375ug / ml of mesityl oxide. Accurately measure 5ml and place it in a 20ml headspace bottle, press the cap and seal to obtain the reference solution. Take blank solvent, reference solution, and test solution for headspace injection into the gas chromatograph. The results show that, under the chromatographic conditions of the present invention, the blank solvent does not interfere with the determination. The resolut...

Embodiment 3

[0047] Example 3 Method system suitability test

[0048] Take the reference solution of Example 2 for 5 consecutive injections, and the chromatographic data is shown in Table 1 below.

[0049] Table 1 Method system suitability test

[0050]

[0051] The results show that, under the conditions of the method of the present invention, the reference solution was injected 5 times continuously, and the RSD of the benzene peak area was 3.96%, which was less than 10%; the theoretical plate number was 159166, which was greater than 5000; The RSD is 2.20%, which is less than 10%, and the theoretical plate number is 473,617, which is greater than 5000, which proves that the method of the present invention has good system applicability.

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Abstract

The invention provides a method for detecting the content of residual solvent benzene and isopropylidene acetone in Avanafil, which comprises the steps of solution preparation and gas chromatography detection. The preparation the test sample solution includes the steps of weighing a test sample, placing the test sample in a volumetric flask, adding N- methyl pyrrolidone (NMP), strongly shaking todissolve, then diluting by water to a scale, and shaking well. The method has the advantages that the separation degree between each target peak to be detected and the adjacent impurity peak is high,there is no mutual interference, and accurate detection for benzene and isopropylidene acetone can be simultaneously realized. In addition, the method is simple and convenient to operate, easy to control and low in detection cost, and has good linear relationship, specificity, system applicability, sensitivity and high added sample recovery.

Description

Technical field [0001] The invention relates to avanafil, in particular to a method for detecting benzene and mesityl oxide residues in avanafil by gas chromatography, and belongs to the technical field of drug analysis. Background technique [0002] Avanafil (Avanafil), chemical name 4-[(3-chloro-4-methoxybenzyl)amino]-2-[2-(hydroxymethyl)-1-pyrrolidinyl]-N- (2-pyrimidinylmethyl)-5-pyrimidine methanesulfonamide is a highly selective inhibitor of phosphodiesterase 5 (PDE5). Compared with other PDE5 inhibitors, avanafil is used to treat male erectile dysfunction (ED), with a faster onset time, which can take effect within 15 to 30 minutes, and the effect is not affected by eating, and the side effects are lower. In the preparation process, avanafil will use organic solvents such as ethanol and acetone, and the organic solvents such as ethanol and acetone in the laboratory have the possibility of containing benzene residue; and acetone has the potential to be derived into mesityl ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/68
CPCG01N30/02G01N30/06G01N30/68G01N2030/042
Inventor 周伟李孝江袁开超周翼马永涛
Owner 重庆瑞泊莱医药科技有限公司
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