FIELD: biology and toxicological chemistry.
SUBSTANCE: method of determining nifedipine in biological material is disclosed, in which a mixture of acetone-acetonitrile in a ratio of 7.5:2.5 by volume is used as an organic isolating agent, before chromatography in a macrocolumn with Silasorb S-18 sorbent 30 mc the residue is dissolved in a mixture of acetonitrile-water solvents in a ratio of 6:4 by volume, during chromatography in a macrocolumn with Silasorb S-18 sorbent 30 mc a two-component mobile phase of acetonitrile-water is used in a ratio of 6:4 by volume; before determination by the physicochemical method, the residue is dissolved in methanol; the chromatography-mass spectrometry method is used as a physicochemical method; when used, it is chromatographed in an HP-5 ms column Ultra Inert 30 m long, with an internal diameter of 0.25 mm, containing a stationary phase, which is (5% phenyl)methylpolysiloxane in the form of a film 0.25 mcm thick, helium is used as the mobile phase, supplied at a rate of 1 ml/min. The detector is a mass spectrometer operating in electron impact mode, the initial temperature of the column thermostat is 70°C, this temperature is maintained for 2 minutes, then the temperature rises from 70 to 200°C at speed 40°C per minute, then from 200 to 290°C at speed 12.5°C per minute, the final column temperature is maintained for 2 min, the injector temperature is 250°C, quadrupole temperature 150°C, detector interface temperature 290°C, record the intensity of the signal caused by charged particles formed when the analyte, released from the capillary column and entering the ion source, is bombarded with an ionizing beam of electrons with an energy of 70 eV, record the mass spectrum from the total ion current and calculate the amount of nifedipine from the area of the chromatographic peak.
EFFECT: invention improves the sensitivity of the analysis.
1 cl, 4 tbl, 3 ex
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Authors
Dates
2024-01-30—Published
2023-06-21—Filed