METHOD FOR QUANTITATIVE DETERMINATION OF GLYPHOSATE, ITS METABOLITE AND GLYPHOSINATE IN ANIMAL PRODUCTS Russian patent published in 2022 - IPC G01N30/06 G01N30/72 G01N30/78 

FIELD: analytical chemistry.

SUBSTANCE: invention relates to the field of analytical chemistry. A method for the quantitative determination of glyphosate, aminomethylphosphonic acid (AMPA) and glufosinate in animal products is disclosed, including the extraction of the analyzed compounds from a sample with deionized water acidified with sulfosalicylic acid, with a subsequent stage of SPP on a reversed-phase sorbent and derivatization with liquid-liquid extraction with diethyl ether, followed by concentration of the inorganic part of the resulting mixture and an additional stage of SPP on a reversed-phase sorbent with weak cation exchange properties, followed by concentration of eluate and its normalization to 1 cm³ before analysis by high-performance liquid chromatography in combination with tandem mass spectrometry. At the same time, 1% sulfosalicylic acid is used as an extractant, and the solid-phase purification (SPP) procedure preceding derivatization is carried out on a cartridge with a reversed-phase sorbent of the Oasis HLB Waters brand 60 mg, 3 cm³, derivatization is carried out at 50°C for 20-45 minutes, and the removal of the residue of the derivatizing agent is carried out by its transfer to diethyl ether with subsequent concentration of the inorganic part of the resulting mixture and additional SPP on a reversed-phase sorbent with weak cation-exchange properties, Oasis WCX Waters, 60 mg, 3 cm³ with additional washing with 1.5 cm³ of 5% formic acid with 20-30% methanol, and subsequent concentration of eluate with its normalization to 1 cm³ before analysis by high-performance liquid chromatography in combination with tandem mass spectrometry.

EFFECT: invention provides the possibility of simultaneous quantitative determination of glyphosate, AMPA and glufosinate, increasing the relative signal intensity of the measuring instrument by increasing the completeness of derivatization and reducing noise from the use of an additional step of the SPP.

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