Development and validation of a UPLC-MS/MS method for the simultaneous estimation of Ertugliflozin and Sitagliptin in bulk and tablet dosage forms: Assessment of greenness and blueness
Voohitha Manukonda, Santhoshi Priya Dandamudi, Praveen Kumar Kusuma, Gouthami Thumma, Kiran Gangarapu
Abstract
• UPLC-MS/MS method was validated for Ertugliflozin and Sitagliptin. • Environmental sustainability was assessed using AES, complexGAPI, and AGREE tools. • The method was practicality evaluated using the BAGI blueness tool. • The method is recommended for routine quality control in pharmaceutical labs. Today, analysts prioritize environmental considerations when creating new analytical methods. Green analytical chemistry emphasizes the use of energy-efficient instruments, minimization of hazardous substances, and reduction of waste. Recent advancements in analytical techniques include the development of compact sample preparation tools, solvent-free extraction methods, and safer solvents. Tools such as the Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical Greenness Metric Approach (AGREE), and practicality/blueness by BAGI assist in evaluating the sustainability of the analytical methods. The primary aim of this study was to develop and assess a sensitive, accurate, and precise UPLC-MS/MS method for simultaneously measuring ertugliflozin (ERT) and sitagliptin (SIT) in bulk and combined tablet forms and to evaluate the greenness profile. The separation was performed on an Agilent ZORBAX® Eclipse XDB-C18 (50 × 2.1 mm, 5 µm) column using the mobile phase of acetonitrile and 2 mM ammonium formate (85:15 v/v) at a flow rate of 0.1 mL/min with isocratic elution, taking 2.5 min per sample. The method was validated for linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The tandem mass spectrometer identified m/z 437.36/415.41 for ERT and m/z 408.11/235.05 for SIT in multiple reaction monitoring (MRM) in positive ionization mode using electrospray ionization (ESI). A linearity range was established for ERT 5–22.5 ng/ml and SIT 10–150 ng/ml with an r² value greater than 0.99. Precision data shows that the % RSD values of ERT and SIT were 0.83 and 1.14 respectively. The % recovery of ERT and SIT was found to be in the range of 98–104.9%. The outcomes of the proposed method were validated and deemed acceptable according to the ICH and USFDA guidelines, successfully allowing simultaneous quantification of the two pharmaceutical compounds.