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Method using liquid chromatography to analyze purity of solid sodium dimethyl dithiocarbamate

A technology of liquid chromatography and formex, which is applied in the field of instrument analysis, can solve the problems of impurity peaks not being detected, peak shape not sharp enough, main peak peak low, etc., to reduce or eliminate peak tailing phenomenon, normal peak, peak shape sharp effect

Inactive Publication Date: 2018-11-27
青岛中科荣达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The solid formamic sodium sample needs to be derivatized before liquid phase analysis. If derivatization is not performed and liquid phase analysis is performed, the peak of the main peak will be low, the peak shape will not be sharp enough, the main peak will be severely tailed, the peak shape will be asymmetrical, and some impurities will The peak cannot be detected, and the detection time is long

Method used

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  • Method using liquid chromatography to analyze purity of solid sodium dimethyl dithiocarbamate
  • Method using liquid chromatography to analyze purity of solid sodium dimethyl dithiocarbamate
  • Method using liquid chromatography to analyze purity of solid sodium dimethyl dithiocarbamate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Instrument:

[0033] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0034] (2) Column Kromstar C18 4.6×250mm 5μm

[0035] (3) Constant temperature column box: Ripley RPL-C2000

[0036] (4) Ultrasonic degassing device.

[0037] 2. Detection conditions:

[0038] (1) Mobile phase: a. 50mmol / L sodium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume fraction). b. Methanol (chromatographic grade). Mobile phase ratio V a :V b =60:40;

[0039] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0040] (3) Flow rate: 0.8mL / min

[0041] (4) Injection volume: 20μL

[0042] (5) Column temperature: 30°C.

[0043] 3. Sample processing:

[0044] Accurately weigh 0.01g of sodium dimethyldithiocarbamate, dissolve it with mobile phase a, set the volume in a 100mL volumetric flask, filter it through an aqueous membrane, and degas it for later use.

[0045] 4. Detection steps: ...

Embodiment 2

[0053] 1. Instrument:

[0054] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0055] (2) Column Kromstar C18 4.6×250mm 5μm

[0056] (3) Constant temperature column box: Ripley RPL-C2000

[0057] (4) Ultrasonic degassing device.

[0058] 2. Detection conditions:

[0059] (1) Mobile phase: a. 50mmol / L sodium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume fraction). b. Acetonitrile (chromatographic grade). Mobile phase ratio V a :V b =70:30;

[0060] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0061] (3) Flow rate: 0.8mL / min

[0062] (4) Injection volume: 20μL

[0063] (5) Column temperature: 30°C.

[0064] 3. Sample processing:

[0065] Accurately weigh 0.01g of sodium dimethyldithiocarbamate, dissolve it with mobile phase a, set the volume in a 100mL volumetric flask, filter through an aqueous membrane, and degas it for later use.

[0066] 4. Detection steps:

...

Embodiment 3

[0075] 1. Instrument:

[0076] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0077] (2) Column Kromstar C18 4.6×250mm 5μm

[0078] (3) Constant temperature column box: Ripley RPL-C2000

[0079] (4) Ultrasonic degassing device.

[0080] 2. Detection conditions:

[0081] (1) Mobile phase: a. 50mmol / L sodium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume); b. Acetonitrile (chromatographically pure);

[0082] Mobile phase ratio V a :V b =70:30, then add 0.2ml of chromatographically pure triethylamine as a pH regulator and tail remover. The addition amount of chromatographically pure triethylamine is mobile phase V a with mobile phase V b two thousandths of the sum of volumes;

[0083] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0084] (3) Flow rate: 0.8mL / min

[0085] (4) Injection volume: 20μL

[0086] (5) Column temperature: 30°C.

[0087] 3. Sample processing...

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Abstract

The invention provides a method using liquid chromatography to analyze the purity of solid sodium dimethyl dithiocarbamate. The method is characterized in that alkaline organic amine compounds are added into the mobile phase. The method using the liquid chromatography to analyze the solid sodium dimethyl dithiocarbamate has the advantages that derivatization treatment is not needed before liquid phase analysis, the pretreatment process is simple, and the method is few in operation steps; all impurity peaks in a sample can be detected, a good separation effect is achieved, peak values are normal, peak shapes are sharp, main peaks without trailing are symmetric in peak shape, and detection time is short.

Description

technical field [0001] The invention relates to a method for analyzing the purity of solid formex sodium by using liquid chromatography, and belongs to the technical field of instrument analysis. Background technique [0002] Sodium furbamate (sodium dimethyl dithiocarbamate) is an important dithiocarbamate. In recent years, sodium fumarate has been used more and more in the sugar making process. The Codex Alimentarius Commission (CAC), the American Food It is a sub-direct food additive approved by the Drug Administration for use in the sugar making process. Due to the pressing, disinfection and sterilization of sugarcane sugar, it can effectively inhibit the growth of bacteria and reduce the resulting sugar loss and other problems. It is used in the sugar making process. It is safe; at the same time, as a fish medicine, it is different from a crop medicine: the fish medicine is splashed on the fish breeding waters, and the medicine directly enters the fish. Generally speak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 郭祥荣王璀杨建民王建亮倪文龙张恭孝郭学阳
Owner 青岛中科荣达新材料有限公司
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