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Method for measuring parachloroaniline content in diflubenzuron

A technology for p-chloroaniline and a determination method is applied in the analysis field of high-performance liquid chromatography for determining the content of p-chloroaniline in diflubenzuron, and can solve the problems of extraction and concentration, and the detection of chloroaniline content has a great influence.

Active Publication Date: 2015-06-03
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But for diflubenzuron, its main component diflubenzuron and the vast majority of impurities produced during the synthesis of diflubenzuron all have peaks in liquid chromatography, and the peak area is much larger than that of p-chloroaniline impurities. It has a great influence on the content detection of chloroaniline
[0007] In addition, the solubility of p-chloroaniline is similar to that of diflubenzuron and other impurities, and solvent extraction and other techniques cannot be used to extract and concentrate to reduce the influence of diflubenzuron and other impurities. Separation is the technical bottleneck, and the difficulty lies in creating a suitable separation method and liquid chromatography conditions to realize the separation of p-chloroaniline from other components and then quantitative determination

Method used

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  • Method for measuring parachloroaniline content in diflubenzuron
  • Method for measuring parachloroaniline content in diflubenzuron
  • Method for measuring parachloroaniline content in diflubenzuron

Examples

Experimental program
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Embodiment 1

[0038] Perform liquid chromatography detection with p-chloroaniline standard solution (300mg / L), and use a diode array (DAD) detector to measure the spectrum, such as figure 1 As shown, p-chloroaniline has strong absorption at 237nm~247nm, especially at 242nm, there is no interference at this wavelength, so 242nm is determined as the detection wavelength.

Embodiment 2

[0040] (1) Preparation of standard solution:

[0041] Standard mother solution: Weigh 0.03g (accurate to 0.0002g) of p-chloroaniline standard substance, dissolve it with acetonitrile in a 100mL volumetric flask, dilute to the mark and shake well. (p-chloroaniline concentration 300 mg / L)

[0042] Standard solution 1: Accurately pipette 1.0mL of the mother solution of the above standard solution into a 100mL volumetric flask and dilute to the mark with acetonitrile and shake well. (p-chloroaniline concentration 3 mg / L)

[0043] Standard solution 2: Accurately pipette 1.0mL standard solution 1 into a 10mL volumetric flask, dilute to the mark with acetonitrile and shake well. (p-chloroaniline concentration 0.3 mg / L)

[0044] (2) Preparation of sample solution

[0045] Weigh about 0.3g (accurate to 0.0002g) of diflubenzuron original drug into a 10mL volumetric flask, add a small amount of dimethylformamide, after ultrasonic dissolution, dilute to the mark with acetonitrile, sha...

Embodiment 3

[0061] According to the detection conditions in Example 2, inject a blank solution after the instrument is stable, and intercept the baseline noise for a period of time N d , and then chromatographically analyze p-chloroaniline standard solution 2 (0.3 mg / L), record the peak response signal H , 3 times the noise is the detection limit, 10 times the noise is the limit of quantification, the detection limit is 0.015mg / L, and the quantification limit is 0.049mg / L.

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Abstract

The invention relates to a method for measuring parachloroaniline content in diflubenzuron. The method comprises sample preprocessing, liquid-phase chromatographic analysis and quantifying by use of an external standard method, wherein the chromatographic conditions are as follows: water serves as a moving phase A, while acetonitrile serves as a moving phase B, gradient eluting is performed at a flow velocity within the range of 0.8-1.2mL / min, and the ratio of the moving phase A is 60-10%, while the ratio of the moving phase B is 40-90%; the detection wavelength ranges from 237 to 247nm. The method is high in specificity, good in degree of precision, and capable of quickly and accurately measuring the parachloroaniline content in the diflubenzuron.

Description

technical field [0001] The invention relates to a method for detecting the content of impurities in pesticides, in particular to an analysis method for measuring the content of p-chloroaniline in diflubenzuron by using high performance liquid chromatography. Background technique [0002] Diflubenzuron, also known as dimetram, or diflubenzuron No. 1, belongs to the class of benzoyl phenylurea insecticides and is an insect growth regulator discovered in the 1970s. The insecticidal mechanism is to inhibit the synthesis of chitin synthase of insects, thereby inhibiting the synthesis of chitin in the epidermis of larvae, eggs, and pupae, so that insects cannot molt normally and die due to deformity, which has a greater impact on crustaceans and silkworms. Toxicity, safe for humans, animals and other organisms in the environment, it is a low-toxic and pollution-free pesticide. The main mode of action is stomach poisoning and contact killing. [0003] In the production process of...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 次素英
Owner HEBEI VEYONG BIO CHEM