Chromatographic and electrophoretic determination of thioamides based on thiazole, 1,3,4-thiadiazole, 1,2,4-triazole,and tetrazole

A procedure was developed for the determination of the following thioamides based on thiazole, 1,3,4-thiadiazole, 1,2,4-triazole, and tetrazole: 2-mercaptothiazole (I), 2-mercapto-1,3,4-thiadiazole (II), 2-mercapto-5-methyl-1,3,4-thiadiazole (III), 3-mercapto-1,2,4-triazole (IV), 3-mercapto-4-methyl-1,2,4-triazole (V), and 5-mercapto-1-methyltetrazole (VI). The determination was performed by reversed-phase HPLC on a column (150 × 4 mm) packed with Diaspher-110-C18 (5 μm) using elution with an acetonitrile-acetate buffer solution (pH 4.70) mixture (5: 95). Detection was performed at the light absorption maximums of compounds I (320 nm), II (305 nm), III (310 nm), IV (260 nm), V (254 nm), and VI (245 nm). The calibration graphs were linear over the following concentration ranges (μg/mL): 0.47–11.72 (I), 0.47–11.82 (II), 0.53–13.22 (III), 0.40–10.11 (IV), 0.46–11.52 (V), and 0.46–11.62 (VI). The limits of detection were 0.45, 0.43, 0.50, 0.37, 0.41, and 0.42 μg/mL for compounds I–VI, respectively. Conditions for the separation of a mixture of compounds I and III–V and for the quantitative determination of compounds I–VI by capillary zone electrophoresis (CZE) were optimized. CZE was performed on a quartz capillary of size 60 cm (effective length of 50 cm) × 75 μm at a voltage of 20 kV with a borate buffer solution (pH 9.18). The procedure allowed us to evaluate the concentrations of substances in the ranges of 1.17–93.75 (I), 1.18–94.54 (II), 1.32–105.76 (III), 1.01–101.13 (IV) 1.15–115.16 (V), and 1.16–116.15 (VI) μg/mL with the detection limits of 1.10, 1.11, 1.20, 0.96, 1.01, and 1.02 μg/mL for compounds I–VI, respectively.