Development and determination of validation parameters for the HPLC method of thymol quantification in “Kalinol plus” syrup
Keywords:validation, “Kalinol plus” syrup, thymol, HPLC
The HPLC method of thymol quantification has been developed for the combined medicine – “Kalinol plus” syrup (produced by “Azerpharm LTD”), which consists of the brotherwort (Thymus serpyllum) extract, sugar syrup, potassium bromide and 80% ethanol. The optimal conditions for quantitative determination of thymol in “Kalinol plus” have been found when carrying out the analysis under different conditions. They are: the flow rate – 1 mL/min, the temperature – 30°C, the volume of injection – 10 μL, the detection wavelength – 274 nm, the type of stationary phase – Zorbax SB-C18 Ø4.6´250 mm, 5 μm, and the mobile phase composition (the mixture of water and acetonitrile (50:50) in the isocratic elution mode), the mass of the sample to be analysed – 1.0 g, the time of analysis – 15 min. It has been found that the analyte peak on the chromatogram is well separated from the peaks of the excipients and other components of the active substance. The validation characteristics of the method proposed have been studied. According to the results obtained the procedure developed is characterised by the acceptable linearity (b = 1.037, a = –5.587, RSD0 = 1.715, Rc = 0.9959), accuracy (δ = 0.16) and precision (Δz = 1.54) in the range of the method application (70-130% of the nominal concentration). Small changes in the flow rate (from 0.8 mL/min to 1.2 mL/min), temperature (from 27°С to 33°С) and the mobile phase composition (from (47:53) to (47:53) ratio) insignificantly affect the values of the symmetry factor of the principal peak, relative standard deviation and the number of theoretical plates. The results of studying stability indicate that the solution to be analysed may be chromatographed within 1 day without losses in accuracy and precision. According to the results the method can be recommended for use in the analysis of “Kalinol plus” syrup.
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