Development and validation of the high-pressure liquid chromatography method for propyltiohinotiadiazol dosage

Abstract

INTRODUCTION. Propylthiohinothiadiazole is a thiadiazole derivative with pronounced antimycobacterial action. Substance is researched in order to develop methods of analysis and standardization, analytical documents regulating quality for use as an active principle in the development of pharmaceutical forms. The purpose. Elaboration of the work technique and validation of the HPLC method for dosing propylthiohinothiadiazole. MATERIAL AND METHODS. 3 series of propylthiohinothiadiazole, internal reference standard of 2-(propylthio)-5H-[1,3,4]- thiadiazole[2,3-b]-quinazolin-5-one substance with concentration 99,98%, chromatographic system Shimadzu LC-20AD HPLC with UV-VIS detector, acetonitrile and dimethylsulfoxide of purity grade “pro HPLC analysis” (Sigma Aldrih and Merck), bidistilled purified water. RESULTS. Linearity is proved for concentrations of 5-30 µg/ml, the linear regression equation is y=36472x44580, R²=0.9929. The limit of detection is 0,729 µg/ml and the limit of quantification is 2,210 µg/ml. It was established that the method is accurate (mean recovery values at 80%, 100% and 120% concentration levels were close to 100%. The accuracy of the method was expressed by repeatability and intermediate accuracy. The variation of the chromatographic conditions established that the method is robust. For all validation parameters, RSD was less than 1. CONCLUSIONS. The validation results show that the developed HPLC method is simple, fast, accurate and reproducible.