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Gas-liquid chromatography is widely used in the process of forensic toxicological examinations, but data about application of GLC with flame-ionization and mass-spectrometry detection for secnidazole determination in analytical toxicology are absent. Aim. To develop GLC/FID- and GLC/MS-procedures for the quantitative determination of secnidazole and carry out step-by-step validation of the procedures developed in the variant of the method of additions. Results and discussion. The chromatographic conditions has been chosen for secnidazole determination by the method of GLC in two variants of performance with flame-ionization and mass-spectrometry detection with the temperature program changing during the analysis from 70 °C to 250 °C or 320 °C. Retention times for secnidazole are 8.97 min and 11.74 min. To prove the possibility of application of the procedures proposed in further analysis their validation has been carried out in the variant of the method of additions. Such validation parameters as in-process stability, linearity, accuracy and precision have been estimated by model solutions. Ex perimental part . The GLC/FID-analysis: HP 6890 Hewlett Packard; НР-1 o0.32 mm × 30 m, 0.25 μm; thermostat – 70 oС (3 min), 40 oС/min to 180 oС (2 min), 40 oС/min to 250 oС (3 min); injector – 280 oС; detector – 280 oС; volume rate of a carrier gas (helium) – 1.5 ml/min; split mode – 1 : 2. The GLC/MS-analysis: Agilent 6890N/5973N/7683; НР-5MS o0.25 mm × 30 m, 0.25 μm; DB-17MS o0.25 mm × 30 m, 0.15 μm; columns are connected sequentially through Deans switch; thermostat – 70 oС (2 min), 45 oС/min. to 210 oС, 6 oС/min to 320 oС (12.56 min); transfer line – 280 oС; ion source – 230 oС; quadrupole – 150 oС; electron impact – 70eV; 40-750 m/z; injector – 250 oС; splitless mode; inlet carrier gas (helium) pressure: 1st column – 26.06 psi, 2nd column – 19.30 psi. Conclusions. New procedures for the quantitative determination of secnidazole by the method of GLC/FID and GLC/MS have been developed. Their validation has been carried out, and acceptability for application has been shown.

Development and validation of GLC/FID- and GLC/MS-procedures of secnidazole determination by the methods of additions