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High performance liquid chromatography method for simultaneously measuring contents of thiophanate methyl and kresoxim-methyl in compound preparation

A technology of high performance liquid chromatography and thiophanate-methyl, which is applied in the field of analysis, can solve the problems of cumbersome sample pretreatment, time-consuming and laborious, etc., and achieve the effect of simple processing, good chromatographic peak shape, and rapid analysis

Active Publication Date: 2014-12-17
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The methods for determining the content of thiophanate-methyl and kresoxim-methyl in the prior art mainly include gas chromatography, complexometric titration, spectrophotometry, etc., wherein the high temperature of the sampling chamber and the chromatographic column in the gas chromatography will destroy the methyl There are two active ingredients of thiophanate and kresoxim-methyl, the process of sample pretreatment in complexometric titration and spectrophotometry techniques is relatively cumbersome, time-consuming and labor-intensive

Method used

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  • High performance liquid chromatography method for simultaneously measuring contents of thiophanate methyl and kresoxim-methyl in compound preparation
  • High performance liquid chromatography method for simultaneously measuring contents of thiophanate methyl and kresoxim-methyl in compound preparation
  • High performance liquid chromatography method for simultaneously measuring contents of thiophanate methyl and kresoxim-methyl in compound preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A batch of thiophanate-methyl and 10% kresoxim-methyl water preparations with marked mass fractions are now produced. 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl aqueous solution were analyzed:

[0032] 1. Detection conditions: Shim pack VP-ODS C18 column: 15cm×4.6mm×5μm, theoretical plate number 3000, mobile phase: methanol:water=75:25 (V / V), wavelength 275nm, column temperature: Room temperature, flow rate: 1ml / min, injection volume: 5 microliters;

[0033] 2. Preparation of standard solution

[0034] Weigh 50.2mg of thiophanate-methyl and 12.5mg of kresoxim-methyl standard samples respectively, add them to a 100ml volumetric flask in turn, add methanol, ultrasonically shake, cool to room temperature after the standard samples are dissolved, and dilute to volume with methanol;

[0035]3. Preparation of sample solution

[0036] Weigh 125mg of labeled mass fraction 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl aqueous solution sample, ...

Embodiment 2

[0044] A batch of marked mass fraction 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl emulsifiable concentrate is now produced. % thiophanate-methyl and mass fraction 10% kresoxim-methyl EC for analysis:

[0045] 1. Detection conditions: Shim pack VP-ODS C18 column: 15cm×4.6mm×5μm, theoretical plate number 3000, mobile phase: methanol:water=60:40 (V / V), wavelength 245nm, column temperature: 40 ℃, flow rate: 1ml / min, injection volume: 5 microliters;

[0046] 2. Preparation of standard solution

[0047] Weigh 50.5mg of thiophanate-methyl and 12.5mg of kresoxim-methyl standard samples respectively, and add them to a 100ml volumetric flask in turn, add acetonitrile, ultrasonically shake, cool to room temperature after the standard samples are dissolved, and dilute to volume with acetonitrile;

[0048] 3. Preparation of sample solution

[0049] Weigh 126 mg of labeled mass fraction 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl EC sample, add to a 100...

Embodiment 3

[0057] A batch of labeled mass fraction 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl microemulsion are now produced. In order to detect the content of active ingredients thiophanate-methyl and kresoxim-methyl, a high performance liquid chromatography analysis method is used to analyze the marked mass fraction 40% thiophanate-methyl and mass fraction 10% kresoxim-methyl microemulsion were analyzed:

[0058] 1. Detection conditions: Agilent ZORBAX C8 column: 25cm×4.6mm×5μm, theoretical plate number 4000, mobile phase: methanol:water=80:20 (V / V), wavelength 250nm, column temperature: 10°C, flow rate : 1ml / min, the injection volume is 5 microliters;

[0059] 2. Preparation of standard solution

[0060] Weigh 50.1mg of thiophanate-methyl and 12.6mg of kresoxim-methyl standard samples respectively, add them to a 100ml volumetric flask in turn, add a mixed solution of n-hexane and dichloromethane with a volume ratio of 1:1, and ultrasonically vibrate to dissolve the ...

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Abstract

The invention belongs to the technical field of analysis and in particular relates to a high performance liquid chromatography method for simultaneously measuring contents of thiophanate methyl and kresoxim-methyl in a compound preparation. According to the method, a 60-80 volume percent of mixed solution of methanol and water in which a mobile phase is methanol is adopted, temperature of a column oven is 10-50 DEG C, flow velocity of the mobile phase is 1ml / min, a sample introduction volume of the sample is 5 micro-liters each time, an impurity peak can be completely separated from a main peak in a detection wavelength range of 245 to 275 nm, the peak shape is good, the integral computation is accurate in result and high in repeatability, the analysis is rapid, the obtained result is high in credibility, the method is particularly suitable for quality control of active ingredients, namely the thiophanate methyl and kresoxim-methyl, in pesticide preparation products, and the production requirements for high-quality compound preparation containing 40 mass percent of thiophanate methyl and 10 mass percent of kresoxim-methyl are met.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a high-performance liquid chromatography analysis method for simultaneously determining the contents of thiophanate-methyl and kresoxim-methyl in compound preparations. Background technique [0002] Thioprazine-methyl is a broad-spectrum systemic and low-toxic fungicide, which can prevent and control various crop diseases. Sheath blight; cotton disease; melon powdery mildew, anthracnose, gray mold; bean gray mold, etc. Kresoxystrobin is a high-efficiency, broad-spectrum, new fungicide, which has good activity against various diseases caused by fungi such as Deuteromycetes, Ascomycetes, Basidiomycetes, Oomycetes, etc. It is effective against grape powdery mildew, potato blight, Rice blast and other diseases, especially for strawberry powdery mildew, melon powdery mildew, cucumber powdery mildew, pear scab. [0003] The compound preparation of thiophanate-methyl and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 吕印美李晓红李太衬姚刚张锐
Owner JINGBO AGROCHEM TECH CO LTD