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Detection method of 3-(1-methylethoxylphosphityl)-propanal

A methyl ethoxyphosphorous acid detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of not knowing the reaction status of the highly toxic raw material sodium cyanide, hidden dangers caused by the safety of material transfer, and reaction Time control is long and other problems, to achieve the effect of stable yield, shorten reaction time, and avoid by-products

Active Publication Date: 2015-11-11
石家庄瑞凯化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a result, the reaction time of this step is controlled for a long time, and the yield is unstable. In addition, the reaction status of the highly toxic raw material sodium cyanide is not understood, which lays hidden dangers for the safety of material transfer.

Method used

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  • Detection method of 3-(1-methylethoxylphosphityl)-propanal
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  • Detection method of 3-(1-methylethoxylphosphityl)-propanal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 detection method

[0050] A kind of detection method of 3-(1-methylethoxyphosphite)-propanal, specifically as follows: its key technology is, it comprises the following steps:

[0051] (1) Preparation of standard products

[0052] 50 g of 3-(1-methylethoxyphosphorous)-propionaldehyde standard substance was added to an excess of 2,4-dinitrophenylhydrazine acidic solution for reaction to obtain a solid product of 3-(1-methylethane Oxyphosphoryl)-2,4-dinitrophenylhydrazone was dried, and the liquid chromatography area normalized quantity was 99.0%.

[0053] (2) Standard solution preparation

[0054] Accurately weigh about 0.1g (accurate to 0.0002g) of the standard sample into a 50ml volumetric flask, dissolve in acetonitrile, dissolve in the mobile phase, dilute to volume, and shake well for later use.

[0055] (3) Sample solution preparation

[0056] Accurately weigh about 0.1g (accurate to 0.0002g) of the mixture sample containing 3-(1-methylethoxyphosph...

Embodiment 2

[0073] Embodiment 2 Quantitative determination methodological verification

[0074] Take 4ml of 2,4-dinitrophenylhydrazine acetonitrile solution, accurately take the solution containing 0.1g of 3-(1-methylethoxyphosphite)-propionaldehyde to be reacted, add it to the same 25ml volumetric flask, and react at 60°C 6min, add mobile phase to constant volume, wavelength 365nm, mobile phase: acetonitrile+water=55+45, external standard method for quantification. See the table below for details:

[0075] Table 1 recovery rate

[0076] the batch

Amount added (mg)

Measured value (mg)

Recovery rate(%)

1

25.5

26.1

102.4

2

37.2

36.9

99.1

3

50.5

49.0

97.1

4

65.1

67.1

103.1

5

77.6

76.2

98.2

[0077] Table 2 Precision

[0078]

[0079] Table 3 Linear correlation test data

[0080] serial number

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Abstract

The invention relates to a detection method of 3-(1-methylethoxylphosphityl)-propanal, wherein the method includes the following steps: (1) preparing a 3-(1-methylethoxylphosphityl)-2,4-dinitrophenylhydrazone standard substance; (2) preparing a 3-(1-methylethoxylphosphityl)-2,4-dinitrophenylhydrazone standard substance solution; (3) preparing a 3-(1-methylethoxylphosphityl)-propanal sample solution; (4) performing HPLC assay; and (5) calculating the mass content of the 3-(1-methylethoxylphosphityl)-propanal through an external standard method. The invention provides the detection method of 3-(1-methylethoxylphosphityl)-propanal, wherein the 3-(1-methylethoxylphosphityl)-propanal is derived by means of 2,4-dinitrophenylhydrazine and the derivative is detected through HPLC. The method is proved to be stable and reliable after method experiment.

Description

technical field [0001] The invention relates to a detection method of 3-(1-methylethoxyphosphorous)-propionaldehyde, in particular to a direct derivation liquid chromatography method for detection of 3-(1-methylethoxyphosphorous) )-propionaldehyde method. Background technique [0002] Agricultural herbicides have brought many advantages to agricultural production, reduced the labor intensity of farmers, effectively controlled the growth of weeds in farmland, and improved the yield and quality of crops. [0003] Glufosinate-ammonium, as a high-efficiency and low-toxicity agricultural herbicide, was developed and produced by the German Hearst Company in the 1980s. Its chemical name is 4-[hydroxyl (methyl)phosphono]-DL-homoalanine (I) . [0004] [0005] Glufosinate-ammonium (I) is a large-tonnage pesticide variety in the world and the second largest herbicide-tolerant transgenic crop in the world. It is easy to degrade in soil, safe for crops, not easy to drift, has a wid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 许丽王收强张明亮
Owner 石家庄瑞凯化工有限公司
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