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High-performance liquid chromatography method for determining content of flumioxazin in flumioxazin crude chemical

A technology of high performance liquid chromatography and prochlorfenazone is applied in the field of pesticide analysis to achieve the effects of good linearity and recovery rate, accurate content determination results and high precision

Inactive Publication Date: 2019-06-14
LIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Except for the assay method in "Handbook of Pesticide Analysis" (Edited by Chen Tiechun et al., Chemical Industry Press, 1st edition, p479-481), there is no other method for the determination of the content of flurachlor propargyl in the technical product of flurafen propargyl. It has been reported in the literature that in order to ensure the quality of the R&D and production of flufenfluzamide preparations, it is necessary to control the content of the original drug

Method used

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  • High-performance liquid chromatography method for determining content of flumioxazin in flumioxazin crude chemical
  • High-performance liquid chromatography method for determining content of flumioxazin in flumioxazin crude chemical
  • High-performance liquid chromatography method for determining content of flumioxazin in flumioxazin crude chemical

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Experimental program
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Effect test

preparation example Construction

[0056] a. Preparation of standard solution:

[0057] Get the standard product of flufenamide propargyl, add acetonitrile to be mixed with the standard product solution of serial concentration;

[0058] b. Determination of standard solution:

[0059] The standard solution of serial concentration is injected into the high-performance liquid chromatograph to detect respectively, and the peak area of ​​the chromatogram is measured, and the standard curve of flufenazol is obtained;

[0060] The chromatographic conditions are as follows:

[0061] Chromatographic column: C18 chromatographic column;

[0062] Detection wavelength: 254±10nm;

[0063] Mobile phase: mobile phase A is phosphoric acid aqueous solution with a volume concentration of 0.1-0.3%; mobile phase B is acetonitrile; the volume ratio of mobile phase A to mobile phase B is 55-40:45-60, and the elution method is isocratic elution;

[0064] (2) Determination of the content of flufenazol propargyl in the sample to be te...

Embodiment 1

[0080] Embodiment 1: the selection of high performance liquid chromatography condition

[0081] 1.1. Selection of mobile phase ratio

[0082] The mobile phase composition of different volume ratios (the proportion of acetonitrile is 45%, 52%, 60% and 65%) is tested, when the proportion of acetonitrile is 60%, 65%, the main peak and the impurity before the main peak come out faster, Can not achieve good separation, the higher the proportion of acetonitrile, the faster the main peak peak, but the worse the separation effect, see respectively image 3 , Figure 4 ; When the proportion of acetonitrile is 45%, the separation effect of the main peak and the impurities in front of the main peak is good. figure 1 ; when the acetonitrile ratio was 52%, the main peak and the impurities before the main peak came out faster, and each component could achieve baseline separation, and the impurities behind the main peak could all appear, see figure 2 .

[0083] In summary, 52% volume ra...

Embodiment 2

[0090] Embodiment 2: the comparison of the method for measuring the content of fluorenzine propargyl

[0091] "Handbook of Pesticide Analysis" Determination method of flufenamide propargyl: Chromatographic column: Zorbax SB-C18, 250mm×4.6mm, particle size 5um, mobile phase is acetonitrile: water = 60:40 (V / V), flow rate: 1.0 mL / min, column temperature: 30°C, detection wavelength: 292nm, injection volume: 5μL.

[0092] Using the same chromatographic column, the "determination method" of the present invention and the determination method on the "Pesticide Analysis Handbook" are compared with the prodrug flufenamide. Although the determination method in the "Handbook of Pesticide Analysis" has a relatively fast time for the main peak to erupt, the impurities cannot all reach the baseline separation, and an inverted peak appears in about 2 minutes; and the wavelength is 292nm, and individual impurities cannot be detected, see Figure 13 .

[0093] In comparison, although the mai...

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Abstract

The invention discloses a high-performance liquid chromatography method for determining the content of flumioxazin in a flumioxazin crude chemical, and belongs to the technical field of farm chemicalanalysis. For making up for the blank of determining the content of the flumioxazin crude chemical at present, the invention provides the high-performance liquid chromatography method for determiningthe content of the flumioxazin in the flumioxazin crude chemical. Under the conditions that a C18 column is taken as a chromatographic column, a mobile phase is acetonitrile (A) and a 0.2% phosphoricacid aqueous solution (B) with a ratio of 52 to 48 (V / V), the flow rate is 1.3mL / min, the column temperature is 40 DEG C and the detection wavelength is 254nm, a standard curve is drawn and a sample to be detected is detected. The method disclosed by the invention is high in precision, high in linearity and recovery rate and accurate in content determination result, can be used for quality controlof the flumioxazin crude chemical to meet the requirements of research development and production, and provides necessary technical support for flumioxazin quality evaluation.

Description

technical field [0001] The invention belongs to the technical field of pesticide analysis, and in particular relates to a high-performance liquid chromatography method for determining the content of flumechlor propargyl in the original drug of flumechlor propargyl. Background technique [0002] Flumioxazin propargyl, the English name is flumioxazin, the trade name is Sumisoya, quick harvest, etc., the chemical name is N-(7-fluoro-3,4-dihydro-3-oxo-(2-propynyl)-2H -1,4-Benzoxazin-6-yl)cyclohex-1-ene-1,2-dicarboximide, a peptidimide herbicide, soluble in most organic solvents , is easy to degrade in the environment, has the characteristics of low toxicity and high efficiency, and good broad-spectrum weed control, and is widely used in agricultural production. The structure of flufenamide propargyl is as follows: [0003] [0004] Flufluramid propargyl usually uses 2,4-difluoronitrobenzene as a starting material, and in the presence of a catalyst, undergoes nitration, ethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/30
Inventor 黄栋李雪梅
Owner LIER CHEM CO LTD
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