Analysis Of Isoxaflutole Product And Its Residue Detection Method In Corn

Isoxaflutole was developed by Rhone – Poulenc.It is an efficient and low toxicity of organic heterocyclic herbicide.The study is divided into the following two parts.1,The qu alitative and quantitative analysis of raw materials,intermediates and target products of isoxazolone was established.The 4-chloro-3-nitro-trifluorotoluene was used as the starting material to synthesize the target product in seven steps.This study analyzed 16 raw materials,6 intermediates and one target product,16 raw materials,of which 4 raw materials(4-chloro-3-nitro-trifluorotoluene,nitroethane,DBU and methyl cyclopropanate)qualitative retention time with the same gas chromatographic conditions,using area normalization method for quantitative acceptance;The raw materials of sodium methanethiol were tested by chemical analysis;The other 11 raw materials according to the current standard for accepting.The1-(2-nitro-4-trifluoromethyl)-1-Nitroethane(Zole01),1-[2-(methylthio-4-trifluoromethyl)phenyl]-3-cyclopropyl-2-acetylmethylenepropane-1,3-dione(Zole05)and5-Cyclopropyl-4-[2-methylthio-4-(trifluoromethyl)benzoyl] isoxazole(Zole06)only studied with control method to determine the reaction rate of the conversion process and then directly to the next step,Sothere is no quantitative analysis method.The analysis of this subject mainly established quantitative analysis methods for three important intermediates2-nitro-4-trifluoromethylacetophenone(Zole02),2-methylthio-4-trifluoromethy lacetophenone(Zole03),1-Cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)propan-1,3-dione(Zole04)and isoxaflutole,Test by method test,the precision and accuracy of the analytical methods meet the analytical requirements,and can meet the requirements of the process conditions to control the reaction process and the quality control of the intermediates and isoxaflutole.The experimental study established a gas chromatographic method for the monitoring of intermediates 1 to 5 and 4 raw materials.2,The establishment of a method of residual analysis of isoxaflutole in corn.After the sample was crushed and mixed,acetic acid and acetonitrile were added,homogenized with a homogenizer and then filtered through a filter paper.Sodium chloride was added to the filtrate to cause severe turbulence and stratification.The acetonitrile solution was extracted with octadecylsilane and graphitized carbon Black purification,in addition to color.The detector was a diode array detector with a detection wavelength of 270 nm.The Agilent C18 column(4.6 mm × 150 mm,5 ?m)was used as the detector.The column temperature was 30 ?,the mobile phase was acetonitrile / water(+ 0.2% HAc)(50:50,V / V),the flow rate was 1.0mL / min and the injection volume was 20?L.The test results showed that the average recoveries of isoxazole from 76.9% to 83.6% and the relative standard deviations(RSDs)from 0.01 to 0.10 mg / kg ranged from 4.2% to 5.9%.The detection methods Isoxaflutole was 0.01 mg / kg.