Method for determining N-methylamino ammate in production of acesulfame

A technique for ammonium acetoacetylsulfamate and a determination method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of incomplete detection chromatographic conditions, low accuracy of measurement data, and inability to accurately measure the content, etc., to achieve improved Product quality, the effect of reducing production costs

Active Publication Date: 2013-04-03
南通宏信化工有限公司
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The Chinese patent application number is 200610085797.5, which discloses a method for measuring the content of ammonium acetoacetamide sulfame ammonium by the area normalization method, but in practi

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  • Method for determining N-methylamino ammate in production of acesulfame

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[0023] (2) Preparation of mobile phase: prepare tetrabutylammonium hydrogensulfate solution with deionized water to a molar concentration of 1.0~2.0mmol / L, prepare tetrabutylammonium hydrogensulfate solution and chromatographic grade methanol by volume ratio of 60:40 to make mobile phase;

[0024] (3) Preparation of the test solution: take an appropriate amount of the sample to be tested, dilute the sample to be tested by volume ratio to a concentration of 0.5% to 2.0% with anhydrous methanol, and prepare a test solution;

[0025] (4) liquid chromatography analysis: draw test solution with micro syringe, inject high performance liquid chromatography, analyze with area external standard method;

[0026] (5) Record the content of ammonium acetoacetylsulfamate in the sample to be tested.

[0027] In actual operation, before the liquid chromatography analysis, the correction factor of the area external standard method is established first, and a complete analysis method of the ar...

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Abstract

The invention discloses a method for determining N-methylamino ammate in production of acesulfame. The method mainly comprises the steps of: (1) selecting an analytical chromatographic condition, an ODS column (4.6mm*25cm) or other equivalent chromatographic columns, wherein the wavelength is 250nm, the flow velocity is 1ml/min, the column temperature is 25 DEG C, and the sample amount is 20mu l; (2) preparing tetrabutylammonium hydrogen sulfate solution from deionized water until the molar concentration is 1.0-2.0mmol/L, and preparing a mobile phase from the prepared tetrabutylammonium hydrogen sulfate solution and chromatographic grade methanol according to the volume ratio of 60 to 40; (3) diluting the sample to be tested by an organic solvent according to the volume ratio until the concentration is 0.5-2.0%, so as to prepare a test solution; (4) absorbing the test solution by a microinjector, injecting into an efficient liquid chromatograph, and analyzing by an area external standard method; and (5) recording the content of the N-methylamino ammate in the sample to be tested. By adopting the method disclosed by the invention, the content of the N-methylamino ammate can be accurately and rapidly determined.

Description

technical field [0001] The invention relates to a method for determining the intermediate ammonium acetoacetylsulfamate in the production of acesulfame potassium. Background technique [0002] At present, the production process of the sweetener acesulfame potassium (trade name: acesulfame potassium) is as follows: the first step reaction uses dichloromethane as a solvent to synthesize ammonium acetoacetylsulfame potassium from sulfamic acid, triethylamine and diketene ; The second step of the reaction is to synthesize acesulfame potassium with acetoacetylsulfame ammonium and sulfur trioxide sulfonated ring; finally neutralize acesulfame acid and potassium hydroxide to obtain acesulfame potassium, that is, acesulfame potassium. [0003] U.S. Patent Application No. 5011982 and 5103046 mentioned in the patent documents that in the production process of the sweetener acesulfame potassium, ammonium acetoacetamide sulfamate is an important intermediate, but only ammonium acetoacet...

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Application Information

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IPC IPC(8): G01N30/02
Inventor 夏秋霞陈小萍汪清玲刘纪才
Owner 南通宏信化工有限公司
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