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Method for detecting content of chloride ions in cyclobenzaprine hydrochloride

A technology for cyclobenzaprine hydrochloride and chloride ion content, applied in the field of chemical analysis, can solve problems such as measurement interference, inapplicable chloride ion content, sediment adhesion, etc., and achieve the effects of eliminating interference, fast and effective measurement, and accelerated dissolution

Active Publication Date: 2021-11-23
NOVAST LABORATORIES (CHINA) LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Using the relationship model between the chloride ion content and absorbance in the suspension, the determination of the chloride ion concentration in the solution is realized, but this method is not suitable for the determination of the chloride ion content in cyclobenzaprine hydrochloride
[0004] CN109212002A discloses a method for detecting chloride ions in nicotinic acid by potentiometric titration, comprising the following steps: weighing a nicotinic acid sample into a beaker, adding deionized water, dissolving in ultrasonic, and filtering to capacity with medium-speed qualitative filter paper Shake at constant volume; pipette 50mL sample solution from the volumetric flask into a beaker, add 0.5mL nitric acid solution, put the rotor in and fix it on a magnetic stirrer, adjust the acidity meter to the potential position, and use a silver electrode as the Indicating electrode, double-salt bridge saturated calomel electrode as reference electrode, titrate with silver nitrate standard solution, record the consumption volume V and potential value E every 0.05-0.1mL, and the titration ends when the potential indicator reaches 350; During the titration process, there will be a problem that the precipitate will adhere to the electrode, which will interfere with the determination.
Specifically: after mixing 1-5g of admixture with 5-10mL of nitric acid solution, 100-300mL of deionized water and 0.5-1mL of ethylene glycol solution, ultrasonically dissolve it for 5-10min; add starch solution, and use a silver electrode as an indicating electrode, The calomel electrode is used as a reference electrode, and the same volume of sodium chloride standard solution is added twice, and the silver nitrate solution is used for titration to the end point under stirring conditions, and the volume of the silver nitrate solution consumed at the end point of the two titrations is respectively obtained; through the blank test Titration obtains the volume of silver nitrate solution consumed and the concentration of silver nitrate solution at the end point of the two titrations; calculates the content of chloride ions in the admixture; in this method, precipitates will adhere to the electrode during the titration process, thereby affecting the determination. interference problem

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  • Method for detecting content of chloride ions in cyclobenzaprine hydrochloride

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Embodiment 1

[0050] The present embodiment provides a method for detecting chloride ion content in cyclobenzaprine hydrochloride, and the method specifically includes the following steps:

[0051] (1) Preparation of test sample: transfer about 200 mg of cyclobenzaprine hydrochloride batch 1 to a suitable beaker, add 200 mL of water to the beaker, stir with a magnetic stirring bar until dissolved, add 5 mL of nitric acid and 4 mL of Triton X-100 solution (5wt%) to obtain the test sample solution;

[0052] (2) Potentiometric titration analysis: adopt the silver nitrate solution of 0.1mol / L to carry out titration to the described test sample solution, and obtain chloride ion content by calculation;

[0053] Among them, the electrode is a composite silver ring smart electrode DMi141-SC, the reference electrolyte is 1 mol / L potassium nitrate solution, the stirring speed is 30%, and the end point recognition threshold is 100 mV / mL.

Embodiment 2

[0055] The present embodiment provides a method for detecting chloride ion content in cyclobenzaprine hydrochloride, and the method specifically includes the following steps:

[0056] (1) Preparation of test sample: transfer about 200 mg of cyclobenzaprine hydrochloride batch 2 into a suitable beaker, add 200 mL of water to the beaker, stir with a magnetic stirring bar until dissolved, add 6 mL of nitric acid and 3 mL of Triton X-100 solution (5wt%) to obtain the test sample solution;

[0057] (2) Potentiometric titration analysis: adopt the silver nitrate solution of 0.1mol / L to carry out titration to the described test sample solution, and obtain chloride ion content by calculation;

[0058] Among them, the electrode is a composite silver ring smart electrode DMi141-SC, the reference electrolyte is 1 mol / L potassium nitrate solution, the stirring speed is 40%, and the end point recognition threshold is 100 mV / mL.

Embodiment 3

[0060] The present embodiment provides a method for detecting chloride ion content in cyclobenzaprine hydrochloride, and the method specifically includes the following steps:

[0061] (1) Preparation of test sample: transfer about 200 mg of cyclobenzaprine hydrochloride batch 1 to a suitable beaker, add 200 mL of water to the beaker, stir with a magnetic stirring bar until dissolved, add 5 mL of nitric acid and 4 mL of polyethylene glycol alcohol to obtain the test sample solution;

[0062] (2) Potentiometric titration analysis: adopt the silver nitrate solution of 0.1mol / L to carry out titration to the described test sample solution, and obtain chloride ion content by calculation;

[0063] Among them, the electrode is a composite silver ring smart electrode DMi141-SC, the reference electrolyte is 1 mol / L potassium nitrate solution, the stirring speed is 40%, and the end point recognition threshold is 100 mV / mL.

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Abstract

The invention provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride. The method for detecting the content of chloride ions in cyclobenzaprine hydrochloride comprises the following steps: (1) preparing a sample to be tested: mixing cyclobenzaprine hydrochloride, nitric acid, a nonionic surfactant and water to obtain a sample solution to be tested; and (2) potentiometric titration analysis: titrating the sample solution to be tested by adopting a silver nitrate solution, and calculating to obtain the content of chloride ions. The test sample is analyzed by adopting a potentiometric titration method, and a titration end point is determined through potential change. The method has the advantages of being high in accuracy, rapid in analysis, high in anti-interference performance and high in sensitivity.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a method for detecting chloride ion content in cyclobenzaprine hydrochloride. Background technique [0002] Chloride ion is a common inorganic anion, but if the concentration is too high, it will also cause certain harm. Therefore, controlling the content of chloride ion is an important item in the quality control of APIs. There are four common detection methods for chloride ions: (1) silver nitrate titration; (2) mercury nitrate titration; (3) potentiometric titration; (4) ion chromatography. Among them, method (3) is suitable for the determination of colored and turbid liquids. The composite silver ring smart electrode is used as the electrode, and the silver nitrate standard solution is used as the titrant. In the titration process, with the continuous addition of titrant, the chloride ion concentration changes continuously, and the potential of the elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N27/26
CPCG01N31/164G01N27/26
Inventor 徐志红陆春晓顾春香胡成松
Owner NOVAST LABORATORIES (CHINA) LTD
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