CN103018368B

CN103018368B - Method for determining N-methylamino ammate in production of acesulfame

Info

Publication number: CN103018368B
Application number: CN201210545067.4A
Authority: CN
Inventors: 夏秋霞; 陈小萍; 汪清玲; 刘纪才
Original assignee: SUZHOU HAOBO TECHNOLOGY HOLDINGS Co Ltd
Current assignee: SUZHOU HAOBO TECHNOLOGY HOLDINGS Co Ltd; Suzhou Hope Technology Co Ltd
Priority date: 2012-12-17
Filing date: 2012-12-17
Publication date: 2014-08-27
Anticipated expiration: 2032-12-17
Also published as: CN103018368A

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

The assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production

Technical field

The present invention relates to the assay method of the intermediate acetyl acetamide ammonium sulfamate in acesulfame potassium production.

Background technology

At present, the production technology of sweetener acesulfame potassium (commodity are called acesulfame potassium) is as follows: the first step is reacted taking methylene chloride as solvent, by sulfaminic acid, triethylamine and ketene dimer synthesis of acetyl acetylamino ammonium sulfamate; Second step reaction becomes acesulfame with acetyl acetamide ammonium sulfamate with SO 3 sulfonated cyclization; Finally acesulfame and potassium hydroxide neutralization reaction are obtained to acesulfame potassium, i.e. acesulfame potassium.

Application No. is to mention in the production technology of sweetener acesulfame potassium in 5011982 and 5103046 patent documentation, acetyl acetamide ammonium sulfamate is a kind of important intermediate, but in literary composition, only acetyl acetamide ammonium sulfamate is carried out to structural characterization with nuclear magnetic resonance, do not set up the content assaying method to acetyl acetamide ammonium sulfamate in reactant liquor.In the continuous production of acesulfame potassium, the component concentration of Accurate Determining acetyl acetamide ammonium sulfamate, can monitor producing reaction ratio, and improve the quality of products, reduce production costs etc. had to important meaning.Chinese Patent Application No. is in 200610085797.5 patent documentation, to disclose a kind of method of measuring acetyl acetamide ammonium sulfamate content with area normalization method, but it is incomplete to find in practice to detect chromatographic condition, institute's usable floor area normalization method can not accurately be measured concrete content, and measurement data accuracy is not high.

Summary of the invention

The object of this invention is to provide a kind of assay method of measuring acetyl acetamide ammonium sulfamate in the acesulfame potassium production that process is quick, measurement data accuracy is high.

For achieving the above object, the present invention has adopted following technical scheme.

The assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production, comprises the following steps:

(1) Analysis on Selecting chromatographic condition: ODS post (4.6mm × 25cm) or other equivalent chromatographic column, wavelength 250nm, flow velocity 1ml/min, 25 DEG C of column temperatures, sample size 20ul;

(2) preparation of mobile phase: preparing 4-butyl ammonium hydrogen sulfate solution to volumetric molar concentration with deionized water is 1.0～2.0mmol/L, is to make mobile phase at 60: 40 by volume by the 4-butyl ammonium hydrogen sulfate solution preparing and hplc grade methanol;

(3) preparation of test solution: get testing sample appropriate, with organic solvent, testing sample being diluted to concentration is by volume 0.5%～2.0%, is made into test solution;

(4) liquid-phase chromatographic analysis: draw test solution with micro syringe, inject high performance liquid chromatograph, analyze by area external standard method;

(5) content of the record acetyl acetamide ammonium sulfamate in testing sample of surveying.

Further, the assay method of acetyl acetamide ammonium sulfamate in aforesaid acesulfame potassium production, wherein: before liquid-phase chromatographic analysis, first set up the correction factor of area external standard method, establish its complete area external standard analytical approach; Method is as follows:

(1) preparation of standard solution: three kinds of mark product solution that with absolute methanol, acetyl acetamide ammonium sulfamate are mixed with to 2mg/ml, 5mg/ml and 10mg/ml by mass/volume concentration;

(2) foundation of correction factor: draw respectively mark product solution with micro syringe, inject respectively high performance liquid chromatograph analysis, after the chromatographic peak area of obtained mark product solution is corresponding with mark product weight contained in this mark product solution, carry out three point calibrations, obtain the correction factor of this area external standard method, thereby establish a complete area external standard analytical approach.

Further, the assay method of acetyl acetamide ammonium sulfamate in aforesaid acesulfame potassium production, wherein: the organic solvent in step (three) is absolute methanol.

Further, the assay method of acetyl acetamide ammonium sulfamate in aforesaid acesulfame potassium production, wherein: the test solution volume by volume concentration in step (three) is 1%.

Further, the assay method of acetyl acetamide ammonium sulfamate in aforesaid acesulfame potassium production, wherein: the volumetric molar concentration of 4-butyl ammonium hydrogen sulfate solution is 1.7mmol/L.

Beneficial effect of the present invention: utilize method of the present invention, can in the production run of acesulfame potassium, determine accurately and quickly the content of acetyl acetamide ammonium sulfamate, thereby can monitor the reaction ratio in production run, strong foundation is provided for improving the quality of products, reducing production costs.

Embodiment

In acesulfame potassium of the present invention being produced below in conjunction with specific embodiment, the assay method of acetyl acetamide ammonium sulfamate is further described.

The present invention selects high performance liquid chromatograph, takes suitable liquid phase chromatogram condition, uses certain mobile phase, thereby analyzes the component concentration of acetyl acetamide ammonium sulfamate in material system.Chromatogram analysis method used in the present invention is area external standard method, due to the response difference of liquid chromatograph to different material, so can reflect accurately the content of component to be measured in order to go out peak area, just must be according to the component to be measured of known quantity the peak area under this chromatographic condition, to calculate quantitative correction factor.Correction factor in this liquid chromatography area external standard method can draw through identical chromatographic condition analytical calculation with the standard model of choosing.

In the present invention, the assay method of acetyl acetamide ammonium sulfamate in described acesulfame potassium production, comprises the following steps:

(3) preparation of test solution: get testing sample appropriate, with absolute methanol, testing sample being diluted to concentration is by volume 0.5%～2.0%, is made into test solution;

In practical operation, before liquid-phase chromatographic analysis, first set up the correction factor of area external standard method, establish its complete area external standard analytical approach.Its method is as follows:

(1) preparation of acetyl acetamide ammonium sulfamate standard model: be that in 5011982 and 5103046 patent documentation, the preparation method of disclosed acetyl acetamide ammonium sulfamate prepares acetyl acetamide ammonium sulfamate sample with reference to Application No., and prepared sample is carried out getting standard samples after three recrystallizations.

(2) preparation of standard solution: above-mentioned standard model is accurately weighed after (being accurate to 0.0002g), with absolute methanol, standard model is mixed with to three kinds of mark product solution of 2mg/ml, 5mg/ml and 10mg/ml by mass/volume concentration;

(3) foundation of correction factor: draw respectively mark product solution with micro syringe, the high performance liquid chromatograph injecting respectively taking mobile phase as liquid phase is analyzed, after the chromatographic peak area of obtained mark product solution is corresponding with mark product weight contained in this mark product solution, carry out three point calibrations, obtain the correction factor of area external standard method, thereby establish a complete area external standard analytical approach.

Because the method step of each embodiment is identical, list associated process conditions and the measurement result thereof in each embodiment with the form of list below, in table 1.

Table 1

As seen from the above table, under this chromatographiccondition of choosing, the sample of variable concentrations is analyzed, all can be obtained relevant data, and test solution concentration 1%, 4-butyl ammonium hydrogen sulfate solution concentration is best during at 1.7mmol/L.Because test solution excessive concentration or too lowly easily exceed the critical field of calibration curve and cause bigger error, and from the data result of analyzing, mobile phase separating effect the best that 4-butyl ammonium hydrogen sulfate solution concentration is all prepared when at 1.7mmol/L in the time of 1.0mmol/L and 2.0mmol/L.

Claims

1. the assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production, comprises the following steps:

(1) the ODS post of Analysis on Selecting chromatographic condition: 4.6mm × 25cm, wavelength 250nm, flow velocity 1ml/min, 25 DEG C of column temperatures, sample size 20 μ l;

(2) preparation of mobile phase: with deionized water preparation 4-butyl ammonium hydrogen sulfate solution to volumetric molar concentration be 1.0～2.0mmol/L, by the 4-butyl ammonium hydrogen sulfate solution preparing and hplc grade methanol by volume for 60:40 makes mobile phase;

(5) content of the record acetyl acetamide ammonium sulfamate in testing sample of surveying;

Wherein, before liquid-phase chromatographic analysis, first set up the correction factor of area external standard method, establish its complete area external standard analytical approach; Method is as follows:

(1) preparation of standard solution: three kinds of mark product solution that with absolute methanol, acetyl acetamide ammonium sulfamate are mixed with to 2mg/ml, 5 mg/ml and 10 mg/ ml by mass/volume concentration;

2. the assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production according to claim 1, is characterized in that: the organic solvent in step (three) is absolute methanol.

3. the assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production according to claim 1 and 2, is characterized in that: the test solution volume by volume concentration in step (three) is 1%.

4. the assay method of acetyl acetamide ammonium sulfamate in acesulfame potassium production according to claim 1 and 2, is characterized in that: the volumetric molar concentration of 4-butyl ammonium hydrogen sulfate solution is 1.7mmol/L.