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High performance liquid chromatography detection method for cyanoacetamide

A high-performance liquid chromatography and cyanoacetamide technology, which is applied in the field of high-performance liquid chromatography to detect cyanoacetamide, can solve problems such as lack of detection precision and sensitivity, poor detection stability, and weak retention, and achieve rapid and efficient determination. highly selective effect

Inactive Publication Date: 2014-07-16
SEPAX TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gas chromatography has the problems of poor detection stability and poor reproducibility for content determination
The chemical titration method does not have high detection precision and sensitivity
It has also been reported that a high-performance liquid phase ODS column was used for detection, but due to the high polarity of cyanoacetamide, the retention on the reversed phase ODS column is very weak, and it is difficult to achieve accurate quantification of cyanoacetamide

Method used

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  • High performance liquid chromatography detection method for cyanoacetamide
  • High performance liquid chromatography detection method for cyanoacetamide
  • High performance liquid chromatography detection method for cyanoacetamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Detection of cyanoacetamide standard

[0023] 1. Sample preparation

[0024] Weigh 5.0 mg of cyanoacetamide standard substance, appropriate amount, add 1 ml of acetonitrile to dissolve to prepare a solution with a concentration of 5 mg / ml, filter through a 0.45 μm microporous membrane and set aside.

[0025] 2. Chromatographic conditions:

[0026] Chromatographic column: Polar-Silica (5 μm, 120 ?, 4.6x250mm) with active silica gel as filler

[0027] Mobile phase: Acetonitrile: Chloromethane=60%:40% (volume ratio)

[0028] Flow rate: 1.0ml / min

[0029] Detector: ELSD (temperature: 60 ℃, gas flow rate: 2.0 L / min)

[0030] Column temperature: room temperature

[0031] Injection volume: 10uL

[0032] 3. Test results:

[0033] According to the above chromatographic conditions, cyanoacetamide was detected. Detection spectrum such as figure 1 Shown: cyanoacetamide peaks at 6.386min, and has a good retention effect on this chromatographic column, thus ensuri...

Embodiment

[0036] Example 2 Detection of cyanoacetamide intermediate.

[0037] 1. Sample preparation:

[0038] Weigh 6.0 mg of cyanoacetamide intermediate, appropriate amount, fully dissolve with 1 ml of acetonitrile to obtain a solution with a concentration of 6 mg / mL, and filter through a 0.45 μm microporous membrane for later use.

[0039] 2. Chromatographic conditions:

[0040] Chromatographic column: Polar-Silica (5 μm, 120 ?, 4.6x250mm) with active silica gel as filler

[0041] Mobile phase: Acetonitrile: Chloromethane=60%:40% (volume ratio)

[0042] Flow rate: 1.0ml / min

[0043] Detector: ELSD (temperature: 60 ℃, gas flow rate: 2.0 L / min)

[0044] Column temperature: room temperature

[0045] Injection volume: 10uL

[0046] 3. Test results:

[0047] According to the above-mentioned chromatographic conditions, the detection spectrum of cyanoacetamide intermediate is as follows figure 2 Shown:

[0048] Chromatographic separation parameters are as follows:

[0049] ...

Embodiment 3

[0052] The detection of embodiment 3 cyanoacetamide industrial products

[0053] 1. Sample preparation:

[0054] Weigh 5 mg of cyanoacetamide industrial product, fully dissolve it with 1 ml of acetonitrile to obtain a solution with a concentration of 5 mg / ml, and filter it through a 0.45 μm microporous membrane for later use.

[0055] 2. Chromatographic conditions:

[0056] Chromatographic column: Polar-Silica (5 μm, 120 ?, 4.6x250mm) with active silica gel as filler

[0057] Mobile phase: Acetonitrile: Chloromethane=60%:40% (volume ratio)

[0058] Flow rate: 1.0ml / min

[0059] Detector: ELSD (temperature: 60 ℃, gas flow rate: 2.0 L / min)

[0060] Column temperature: room temperature

[0061] Injection volume: 5uL

[0062] 3. Test results:

[0063] According to the above chromatographic conditions, the detection spectrum of cyanoacetamide industrial products is as follows: image 3 shown.

[0064] Chromatographic separation parameters are as follows:

[0065] ...

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Abstract

The invention provides a high performance liquid chromatography detection method for cyanoacetamide. The chromatographic conditions adopted by the method include that: the chromatographic column is Polar-Silica, the particle size is 5 micrometers, the length is 250mm, the diameter is 4.6mm, and the aperture is 120 angstrom; the mobile phase is a mixed system of acetonitrile and methyl chloride; and the detector is ELSD. The detection method provided by the invention has the advantages of rapidity, accuracy, high selectivity, simple sample treatment, and is suitable for qualitative and quantitative detection of cyanoacetamide industrial crude products and intermediates.

Description

technical field [0001] The invention relates to a method for detecting cyanoacetamide through high-performance liquid chromatography, and belongs to the technical field of analysis. Background technique [0002] Cyanoacetamide is a white powdery crystal, soluble in various organic solvents, soluble in water, poisonous, and is an important intermediate in organic synthesis. Cyanacetamide is obtained from the action of ethyl cyanoacetate and ammonia, and is used in the synthesis of malononitrile and electroplating solutions, and also in the synthesis of drugs such as triamterene and aminopterin. In China, cyanoacetamide is mainly used in the preparation of water treatment agent 2,2-dibromo-3-cyanopropionamide, and is also used in the production of spices and pharmaceutical intermediate β-methylglutaric acid monomethyl ester. The consumption of cyanoacetamide in this field will maintain the current level. [0003] At present, gas chromatography or chemical titration are often...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/36
Inventor 龚立冬李彧娜徐文娟于淑香
Owner SEPAX TECH
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