METHOD FOR DETERMINING HYDROXYLATED POLYCYCLIC AROMATIC HYDROCARBONS IN URINE Russian patent published in 2024 - IPC G01N33/493 G01N30/72 

FIELD: analytical toxicology.

SUBSTANCE: invention can be used in biomonitoring of individuals exposed to polycyclic aromatic hydrocarbons (PAHs) under industrial conditions, namely a method for chromatography-mass spectrometric determination of hydroxylated polycyclic aromatic hydrocarbons in urine. The method for chromatography-mass spectrometric determination of hydroxylated polycyclic aromatic hydrocarbons in urine includes dispersive liquid-liquid microextraction, centrifugation and derivatization of hydroxylated polycyclic aromatic hydrocarbons with a silylation reagent, with additional enzymatic hydrolysis of the sample, β-glucuronidase at 55°C for 1 hour, dispersive liquid-liquid microextraction is carried out by adding internal standard 1-hydroxypyrene-d9, 2 ml of 0.1 M hydrochloric acid, 300 mcl of ethanol, 100 mcl of trichloromethane to the sample, shaking for 25 s to form an emulsion, centrifugation at 5000 rpm for 10 min, the bottom layer is taken into a 250 mcl insert, derivatization is carried out in the chromatograph evaporator with a three-phase system of 1 mcl of the silylation reagent N,O-bistrimethylsilyltrifluoroacetamide, 0.2 mcl of air and 1 mcl of trichloromethane extract, followed by analysis on a capillary column NT-8 in temperature gradient mode for 15 minutes.

EFFECT: above method simplifies sample preparation and promotes more complete extraction of analytes due to dispersive liquid-liquid microextraction (DLLME), which eliminates the evaporation process, silylation in the injection port (evaporator), and reducing the duration of GC-MS analysis on a capillary column. The invention also provides increased selectivity.

1 cl, 3 dwg, 6 tbl