METHOD OF DETERMINING DELTAMETHRIN AND LAMBDA-CYHALOTHRIN IN BIOLOGICAL MATERIAL

摘要

FIELD: chemistry.;SUBSTANCE: biological material is ground, twice in 1 hour infused with dioxane; extractions are merged, filtered and evaporated, diluted 5 times with water, extracted with ethyl acetate twice; the extracts are merged, dehydrated; the solvent is evaporated in an air current and then in a nitrogen current; the residue is dissolved in a mixture of solvents hexane-dioxane-propanol-2 in ratio of 150:5:1, chromatographed in a column with silica gel L 40/100 µ using a hexane-dioxane-propanol-2 mobile phase in ratio of 150:50:1; eluate fractions containing the analyte are merged, the eluent is evaporated in an air current and then in a nitrogen current, the residue is dissolved in hexane and determination is carried out via chromatography-mass spectrometry using a capillary column HP-5 MS 30 m×0.25 mm×0.25 mcm, which contains diphenyl dimethyl polysiloxane and polethylene glycol, using a helium carrier gas which is fed at a rate of 1 ml/min, and a mass-selective quadropole detector operating in electron impact mode with electron energy of 70 eV, while recording the mass-spectrum on total ion current; the initial temperature of 50°C is maintained for 1 minute, and then programmed from 50°C to 200°C at a rate of 50°C/min, from 200°C to 280°C at a rate of 20°C/min, while maintaining the final temperature for 10 minutes; injector temperature is 280°C, interface temperature is 260°C, quadropole temperature is 150°C and ion source temperature is 230°C. The amount of deltamethrin or lambda-cyhalothrin is calculated from chromatograph data.;EFFECT: high sensitivity and selectivity of determination.;4 tbl, 3 ex