Development and Validation of HPLC-DAD and UHPLC-DAD Methods for the Simultaneous Determination of Guanylhydrazone Derivatives Employing a Factorial Design

Abstract

Guanylhydrazones are molecules with great pharmacological potential in various therapeutic areas, including antitumoral activity. Factorial design is an excellent tool in the optimization of a chromatographic method, because it is possible quickly change factors such as temperature, mobile phase composition, mobile phase pH, column length, among others to establish the optimal conditions of analysis. The aim of the present work was to develop and validate a HPLC and UHPLC methods for the simultaneous determination of guanylhydrazones with anticancer activity employing experimental design. Precise, exact, linear and robust HPLC and UHPLC methods were developed and validated for the simultaneous quantification of the guanylhydrazones LQM10, LQM14, and LQM17. The UHPLC method was more economic, with a four times less solvent consumption, and 20 times less injection volume, what allowed better column performance. Comparing the empirical approach employed in the HPLC method development to the DoE approach employed in the UHPLC method development, we can conclude that the factorial design made the method development faster, more practical and rational. This resulted in methods that can be employed in the analysis, evaluation and quality control of these new synthetic guanylhydrazones.

Fragment-based design of α-cyanoacrylates and α-cyanoacrylamides targeting Dengue and Zika NS2B/NS3 proteases

“…Finally, all HPLC R T values were computed in minutes (min), while the absorbance was computed as milli-absorbance unities (mAU). 101,176…”

“…Finally, all HPLC R T values were computed in minutes (min), while the absorbance was computed as milli-absorbance unities (mAU). 101,176 4.11.3 Melting point determination -(mp). An MSTecnopon s (Piracicaba, Brazil), model PFMII Digital, equipment was used to determine the melting point (mp) for each final compound.…”

Computational-Based Study of QuEChERS Extraction of Cyclohexanedione Herbicide Residues in Soil by Chemometric Modeling

“…The aim of the factorial design is to identify the key variables and possible synergistic effects controlling the process [ 21 , 23 ], which allow modeling of the QuEChERS extraction to maximize the recoveries of CHD residues from soil. Bruzzoniti et al [ 24 ] have already highlighted the necessity of using chemometric tools to contribute to a better understanding of the extraction process in soil.…”

“…These optimizations are often performed by sequential analysis of individual variables, which is time consuming and increases the analysis costs [ 12 , 16 , 19 ]. In this context, chemometrics could help overcome these drawbacks, thereby reducing the number of experiments and maximizing the information obtained [ 21 ].…”

Computer-Aided Design, Synthesis, and Antiviral Evaluation of Novel Acrylamides as Potential Inhibitors of E3-E2-E1 Glycoproteins Complex from Chikungunya Virus

“…Moreover, some parameters were established, such as (a) sample concentration of 1 mg/mL; (b) flow of 1 mL/min; (c) run time of 15 min; and (d) injection volume of 5 µL. Finally, the retention times (R T ) were computed in minutes (min) and absorbance, in mili-absorbance unities (mAU) [101].…”