METHOD OF DETECTING ESPHEN VALERATE IN BIOLOGICAL MATERIAL Russian patent published in 2012 - IPC G01N33/48 G01N30/02 

FIELD: medicine.

SUBSTANCE: biological tissue is crushed, twice for 1 hour is drawn with portions of dioxane, each of which by weight is two times the amount of biomaterial, separate extracts are combined, filtered, filtrate is evaporated in air flow at temperature 18-22°C to small volume, diluted 5 times with water, extracted with ethyl acetate, ethyl acetate extract is separated, dehydrated, evaporated at 18-22°C in air flow to small volume, after which in nitrogen flow until solvent is removed completely, residue is dissolved in mixture of solvents hexane-dioxane-propanol-2 (150:5:1), purified by method of column chromatography in column with size 490×11 mm, filled with 10 g of silica gel L 40/100 mc, with application of mobile phase solvents hexane-dioxane-propanol-2 (150:5:1), eluate fraction, which contain analysed substance, combined, eluate is evaporated in air flow at temperature 18-22°C to small volume, then in nitrogen flow until solvent is removed completely, residue is dissolved in hexane and detection is carried out by method of gas-liquid chromatography with application of capillary column DB-1701, 30 m long, with internal diameter 0.25 mm with stationary phase 0.25 mcm thick, which contains polysiloxane and polyethylene glycol, with application of helium as carrier gas, supplied with velocity 1 ml/min and mass-spectrometric detector, working in mode of electron impact, with registration of mass-spectrum by full ion flow, amount of esphen valerate is calculated by data of chromatogram, obtained by registering intensity of signal induced by charged particles formed during bombardment of analysed substance, which comes from capillary column and gets into source of ions, by ionising beam of electrons with energy 70eV.

EFFECT: increase of detection sensitivity.

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