METHOD OF DETERMINING N-BUTYL ETHER OF 2-[4-(5-TRIFLUOROMETHYL PYRIDYL-2-OXY)PHENOXY]PROPIONIC ACID IN BIOLOGICAL MATERIAL Russian patent published in 2013 - IPC G01N33/483 G01N33/52 

FIELD: chemistry.

SUBSTANCE: analysed sample is crushed, twice infused with acetone; the acetone extract is filtered; the solvent is evaporated from the filtrate; the residue is dissolved, purified on a column with a sorbent using as the mobile phase a mixture of solvents; eluate fractions containing the analysed substance are combined and determination is carried out using a physical-chemical technique, where the residue obtained after evaporating the solvent from the filtrate is treated with acetone several times; acetone extracts are separated and combined; the solvent from the combined extracts is evaporated; the residue is purified in a column with a Silasorb S-18 sorbent, using a mobile phase of acetonitrile-water (7:3); after combining the eluate fractions containing the analysed substance, the obtained solution is diluted with water, extracted with diethyl ether; the ether extract is separated, evaporated to a dry residue; the residue is dissolved in hexane and determination is carried out via a chromatographic-mass-spectrometric technique using a capillary column of DB-1MS with length of 30 m and inner diameter of 0.25 mm with a stationary phase with thickness of 0.25 mcm, which is dimethylpolysiloxane, using helium as the carrier gas which is fed at a rate of 39 cm³/s, and a mass-spectrometric detector operating in electron impact mode, with recording of a mass spectrum on total ion current; the amount of n-butyl ether of 2-[4-(5-trifluoromethyl pyridyl-2-oxy)phenoxy]propionic acid is calculated from the chromatogram data obtained by detecting intensity of the signal due to charged particles formed when bombarding the analysed substance, coming out of the capillary column and fed into the ion source, using an ionising beam of electrons with energy of 70 eV.

EFFECT: high sensitivity.

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