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Method for detecting tert-butylamine in arotinolol hydrochloride

A detection method, the technology of tert-butylamine, applied in the field of drug analysis

Inactive Publication Date: 2021-07-23
河北利德检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report about the detection of tert-butylamine in arololol hydrochloride

Method used

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  • Method for detecting tert-butylamine in arotinolol hydrochloride
  • Method for detecting tert-butylamine in arotinolol hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Chromatographic conditions: Chromatographic column: InertCap for Amines, 0.32mm×30m.

[0023] Column temperature: the initial temperature is 60°C, maintained for 13 minutes, then raised to 240°C at a rate of 30°C / min, and maintained for 10 minutes.

[0024] Detector temperature: 250°C.

[0025] Injection port temperature: 150°C.

[0026] Carrier gas: high-purity nitrogen.

[0027] Flow rate: 1ml / min; hydrogen flow rate: 40ml / min; air flow rate: 400ml / min.

[0028] Split ratio: 10:1.

[0029] Injection volume: 1 μl.

[0030] Solution preparation

[0031] Sodium methoxide solution: weigh 2.4g of sodium methoxide, put it in a 50ml volumetric flask, dilute to the mark with methanol, and mix well;

[0032] Preparation of control solution:

[0033] Weigh 16mg of tert-butylamine, put it in a 50ml volumetric flask, and dilute to volume with methanol; accurately measure 1ml from it, place it in a 20ml volumetric flask, and dilute to volume with methanol as a control solut...

Embodiment 2

[0036] Recovery rate control stock solution: Accurately weigh 16mg of tert-butylamine, accurately weigh it, put it into a 50ml volumetric flask, dissolve it with methanol and constant volume, and make the concentration 320μg / ml; recovery rate control stock solution.

[0037] Recovery rate control solution: Take 1ml of recovery rate control stock solution into a 20ml volumetric flask, add methanol to volume.

[0038] Test solution: take about 500mg of alololol hydrochloride, accurately weigh it, add distilled water to dissolve and dilute to 10ml, and make a sample solution with a concentration of 5mg / ml.

[0039] Accuracy solution: take each 500mg of the test product, accurately weigh it into a 10ml volumetric flask, first add 5ml of sodium methoxide solution to completely dissolve the sample, then add the control solution according to 80%, 100%, and 120% of the limit respectively, namely Add recovery control stock solution 0.4ml, 0.5ml, 0.6ml respectively, add methanol to diss...

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Abstract

The invention discloses a method for detecting tert-butylamine in arotinolol hydrochloride. The method is a gas chromatography method, a hydrogen flame ionization detector is provided, the detector is a hydrogen flame ionization detector (FID for short), the temperature is 248-252 DEG C, and the optimal temperature is 250 DEG C; the temperature of a sample inlet is 148-152 DEG C, and the optimal temperature is 150 DEG C; the flow velocity of the chromatographic column is 0.9-1.1 ml / min, and the optimal flow velocity is 1.0 ml / min; the temperature rise procedure of the chromatographic column is as follows: the initial temperature is 60 DEG C, the temperature is maintained for 13 minutes, and then the temperature is raised to 240 DEG C at the rate of 30 DEG C / min and maintained for 10 minutes; direct sample introduction is carried out, and the sample introduction volume is 1 microliter; and the split ratio is 10: 1, and preparation of a test solution comprises that 0.5 g of arotinolol hydrochloride is weighed. The tert-butylamine cannot be detected because the arotinolol hydrochloride reacts with free hydrochloric acid in a solution after the arotinolol hydrochloride is dissolved, however, according to the method, a proper amount of aqueous alkali is added into a sample solution to neutralize the hydrochloric acid so that the purpose of detection is achieved. The method is subjected to complete verification and has the advantages of high sensitivity, good specificity, simplicity in operation and the like.

Description

technical field [0001] The invention relates to a method for detecting tert-butylamine in arololol hydrochloride in the field of drug analysis Background technique [0002] Alolol hydrochloride is a white powder, odorless and tasteless. [0003] Alolol hydrochloride, known as the fourth-generation beta-blocker, is the first-line drug for beta-blockers. Clinically, it is mainly used for the treatment of mild to moderate essential hypertension, angina pectoris, tachycardia arrhythmia, and essential tremor. [0004] The 2020 edition of the "Chinese Pharmacopoeia" does not include the inspection item of tert-butylamine under the variety of arololol hydrochloride, and the detection of tert-butylamine in arololol hydrochloride is not included in the searchable pharmacopoeias such as the United States Pharmacopoeia and the European Pharmacopoeia. There is no report on the detection of tert-butylamine in arololol hydrochloride. [0005] From the structural analysis of alololol hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/16G01N30/30G01N30/32G01N30/68
CPCG01N30/482G01N2030/484G01N30/02G01N30/68G01N30/30G01N30/14G01N30/16G01N30/32G01N2030/324
Inventor 齐盈盈蔡敬凤吴蒙于新娈薛晨光常云飞刘晗
Owner 河北利德检测技术有限公司
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