METHOD FOR QUANTITATIVE DETERMINATION OF CLAVULANIC ACID IN MUSCLE TISSUES OF ANIMAL ORIGIN Russian patent published in 2022 - IPC G01N30/02 G01N33/12 

FIELD: analytical chemistry.

SUBSTANCE: invention relates to the field of analytical chemistry and can be used to control the content of residual amounts of clavulanic acid in animal products. The method for quantitative determination of the content of clavulanic acid in muscle tissues of animal origin (in particular, in the muscle tissues of cattle) includes the extraction of the analyzed compound from the sample with a solution of acetonitrile in deionized water acidified with formic acid, followed by a solid-phase purification (SPF) on reversed-phase sorbent with weak anion exchange properties and subsequent filtration before analysis by high performance liquid chromatography in combination with tandem mass spectrometry. At the same time, the extraction of the analyzed compound from the sample is carried out with a mixture of deionized water and acetonitrile, acidified with formic acid, in a ratio of 90/9.5/0.5. The SPF procedure is carried out on a cartridge of Oasis WAX Waters reverse-phase sorbent (60 mg, 3 cm³), with an additional washing step of 1 cm³ of a mixture of acetonitrile and deionized water, in a ratio of 1/1, and elution of clavulanic acid with 1 cm³ of a mixture of acetonitrile with deionized water and formic acid in a ratio of 49.75/49.75/0.5, followed by filtration before analysis by high performance liquid chromatography in combination with tandem mass spectrometry.

EFFECT: method makes it possible to increase the extraction of the analyte from the objects of study, provides an increase in the relative intensity of the signal of the measuring instrument by reducing noise during the application of the SPF stage, which significantly increases the analytical response of the mass spectrometer detector when determining clavulanic acid in muscle tissues of animal origin and allows for a full-fledged quantitative analysis of this compound.

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