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Method for detecting solid potassium dimethyldithiocarbamate purity by liquid phase chromatography method

A technology of liquid chromatography and thiram potassium, which is applied in the field of instrument analysis, can solve the problems of long peak extraction time, cumbersome operation, asymmetric peak shape, etc., and achieve the effects of small analysis error, high analysis precision and good separation effect

Active Publication Date: 2018-11-06
青岛中科荣达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of anticancer drugs has stricter requirements on the purity of thiram potassium and the structure and content of impurities in thiram potassium. In the prior art, there is a liquid chromatography method for a series of products with a similar structure to thiram potassium, but the operation is cumbersome and purification is required before injection. , Concentration and other pretreatments are time-consuming and labor-intensive, which has been a long-term problem for researchers. If the liquid chromatographic detection is carried out directly after the dissolution of thiram potassium, there will be: the main peak and the impurity peak cannot be well separated, the main peak peak value is low, The peak shape is asymmetrical; the peak time is long; the tailing phenomenon of the main peak is serious

Method used

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  • Method for detecting solid potassium dimethyldithiocarbamate purity by liquid phase chromatography method
  • Method for detecting solid potassium dimethyldithiocarbamate purity by liquid phase chromatography method
  • Method for detecting solid potassium dimethyldithiocarbamate purity by liquid phase chromatography method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Selection of instruments:

[0030] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0031] (2) Column Kromstar C18 4.6×250mm 5μm

[0032] (3) Constant temperature column box: Ripley RPL-C2000

[0033] (4) Ultrasonic degassing device.

[0034] 2. Setting of detection conditions:

[0035] (1) Mobile phase: a. Water (containing 0.05% tetrabutylammonium chloride by volume);

[0036] b. Methanol (chromatographically pure);

[0037] Mobile phase ratio V a :V b =60:40;

[0038] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0039] (3) Flow rate: 0.8mL / min

[0040] (4) Injection volume: 20μL

[0041] (5) Column temperature: 30°C.

[0042] 3. Sample processing:

[0043] Accurately weigh 0.01g of potassium 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.

[0044] 4. Detection steps: ...

Embodiment 2

[0053] 1. Selection of instruments:

[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. Setting of detection conditions:

[0059] (1) Mobile phase: a. 1% potassium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume);

[0060] b. Methanol (chromatographically pure);

[0061] Mobile phase ratio V a :V b =60:40;

[0062] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0063] (3) Flow rate: 0.8mL / min

[0064] (4) Injection volume: 20μL

[0065] (5) Column temperature: 30°C.

[0066] 3. Sample processing:

[0067]Accurately weigh 0.01g of potassium 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 ...

Embodiment 3

[0076] 1. Selection of instruments:

[0077] (1) FL2200 liquid chromatograph with UV detector, N2000 chromatographic workstation

[0078] (2) Column Kromstar C18 4.6×250mm 5μm

[0079] (3) Constant temperature column box: Ripley RPL-C2000

[0080] (4) Ultrasonic degassing device.

[0081] 2. Setting of detection conditions:

[0082] (1) Mobile phase: a. 1% potassium dihydrogen phosphate solution (containing 0.05% tetrabutylammonium chloride by volume);

[0083] b. Acetonitrile (chromatographically pure);

[0084] Mobile phase ratio V a :V b =65:35;

[0085] (2) Detection wavelength: 260nm (determined by a diode array detector)

[0086] (3) Flow rate: 0.8mL / min

[0087] (4) Injection volume: 20μL

[0088] (5) Column temperature: 30°C.

[0089] 3. Sample processing:

[0090] Accurately weigh 0.01g of potassium 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 l...

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Abstract

The invention provides a method for detecting solid potassium dimethyldithiocarbamate purity by a liquid phase chromatography method. According to the method, mobile phases are composed of a mobile phase a, a mobile phase b and a mobile phase c; the mobile phase c is an alkali organic amine compound. Derivation or preprocessing is not needed before liquid phase analysis is conducted on a sample, and sample analysis is directly carried out after dissolving and deaeration are conducted; in an obtained liquid phase chromatogram, all impurity peaks in the sample are detected, the separation effectbetween a main peak and the impurity peaks is good, the peak value is normal, the peak shape of the main peak is symmetric, smearing does not exist, and the detection time is short.

Description

technical field [0001] The invention relates to a method for detecting the purity of solid thiram potassium by liquid chromatography, and belongs to the technical field of instrument analysis. Background technique [0002] The dithiocarbamate derivatives synthesized from thiram potassium (scientific name potassium dimethyl dithiocarbamate) as the starting material can be complexed with copper ions to form complexes, which have antibacterial, antiviral and antitumor properties. biological activity. The synthesis of this anticancer drug has stricter requirements on the purity of Potassium Potassium, the structure and content of impurities in Potassium Potassium. In the prior art, there is liquid chromatography for series products with similar structure of Potassium Potassium Potassium, but the operation is cumbersome and purification is required before injection. , Concentration and other pretreatments are time-consuming and labor-intensive, which has been a long-term problem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 郭祥荣王璀王建亮刘梅王亮倪文龙杨荣华郭学阳
Owner 青岛中科荣达新材料有限公司
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