METHOD OF DETERMINING O-(2,3-DIHYDRO-2,2-DIMETHYL-7-BENZOFURANYL)-N-METHYL CARBAMATE IN BIOLOGICAL MATERIAL Russian patent published in 2015 - IPC G01N33/52 

FIELD: chemistry.

SUBSTANCE: method is carried out as follows: crushing biological material containing O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methyl carbamate, treating the material three times with a mixture of ethyl acetate and acetone taken in ratio of 1:1 by volume, each time for 30 minutes; merging the obtained extracts; evaporating the extractant; dissolving the residue in acetonitrile; diluting the obtained solution with water in ratio of 1:4 by volume; extracting with ethyl acetate twice with volume ratio of water to the organic phase of 1:1 at each extraction step; merging the ethyl acetate extracts; evaporating to a dry residue; dissolving the residue in acetonitrile; adding water to the solution to achieve volume ratio of acetonitrile to water of 4:6; adding the obtained solution to a Silasorb S18 sorbent column; carrying out a chromatographic process using a two-component mobile phase of acetonitrile-water in ratio of 4:6 by volume; merging eluate fractions containing O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methyl carbamate; evaporating the eluent; dissolving the residue in methanol and performing determination with a physical-chemical method, which is chromatography-mass spectrometry, in a DB-5 MS EVIDEX capillary column with length of 25 m and inner diameter of 0.2 mm with a stationary phase which is 5% phenyl-95% methylpolysiloxane, with film thickness of the stationary phase of 0.33 mcm, using a helium carrier gas fed at a rate of 0.6 ml/min, and a mass-selective detector operating in electron impact mode, the initial thermostat temperature of the column being 70°C; maintaining said temperature for 3 min, then raising the temperature from 70°C to 290°C at a rate of 20°C/min; maintaining the final temperature of the column for 16 min; temperature of the injector is 250°C, temperature of the quadrupole is 150°C, temperature of the detector interface is 300°C; detecting strength of the signal resulting from charged particles formed when bombarding the analysed substance coming from the capillary column and falling into an ion source with an ionising electron beam with energy of 70 eV; recording the mass spectrum on the full ion current and calculating the amount of O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methyl carbamate from the area of the chromatographic peak.

EFFECT: high sensitivity.

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