Current Pharmaceutical Analysis - Volume 19, Issue 1, 2023

Background: Dexamethasone (DEXA) is a potent synthetic corticosteroid derived from the cyclopentanoperhydrophenanthrene nucleus known for its anti-inflammatory and immunosuppressive activities. Due to its therapeutic effects, several analytical methods have been used for its quantitative determination and physicochemical characterization, as well as for the evaluation of pharmacological and toxicological properties. Objective: This review aimed to describe the principles and methods commonly used to identify and quantify DEXA in drug delivery systems and biological samples. The methods herein discussed are high-performance liquid chromatography, nuclear magnetic resonance, x-ray diffraction, Fourier-transform infrared spectroscopy, differential scanning calorimetry, ultravioletvisible spectrophotometry and thin layer chromatography. Conclusion: This review provided a wide variety of analytical methods that can be used for the quantification and identification of drugs, providing scientists with great support during the development of scientific research, as well as ensuring the quality of the manufacturing processes as well as the resulting products. Therefore, the use of such analytical methods has become critical throughout the process of developing pharmaceutical formulations containing DEXA.

A new antidiabetic drug combination of Metformin Hydrochloride, Dapagliflozin, and Saxagliptin have been recently approved for type II diabetes. This is marketed by Takeda Pharmaceuticals under the brand name Qternmet XR. Although different analytical and bioanalytical methods using different techniques such as liquid chromatography, high-performance liquid chromatography, high-performance thin-layer chromatography, gas chromatography, spectrophotometry, spectrofluorimetric methods coupled with ultraviolet, fluorescence, mass, or tandemmass spectrometry detection have already been developed for the determination of Metformin Hydrochloride, Dapagliflozin, and Saxagliptin. Sensitive, cost-effective, and more optimized methods are yet required. Therefore, this review summarizes the main analytical and bioanalytical aspects regarding not only simultaneous estimation but also stability-indicating methods, kinetic studies, and impurity analysis for the analysis of proposed drugs in bulk and pharmaceutical dosage forms. Thus, this review gathers, for the first time, important background information on all analytical and bioanalytical methods that have been developed and applied for the determination of Metformin Hydrochloride, Dapagliflozin, and Saxagliptin, which should be considered as a starting point if new techniques are aimed to be implemented for these drugs.

Sofosbuvir is a regularly used antiviral medication that was approved for clinical usage in hepatitis C patients. Sofosbuvir belongs to the nucleotide analog drug class, and it operates by inhibiting hepatitis C NS5B protein. This study focuses on the many analytical methods for detecting and quantifying Sofosbuvir in pharmaceutical formulations, biological samples, and fixed dosage combinations. Chromatographic techniques, electro-analytical methods, chemometric procedures, and optical approaches are just a few of the approaches mentioned in the literature. The most often used methods for the analysis of Sofosbuvir are HPLC-based methods with UV/Vis spectrophotometric, fluorescence, and mass spectrometric detection. This article could be extremely useful in creating upcoming Sofosbuvir analytical approaches or investigations.

Background: Products with multiple active substances mixed in a single dosage form are fixed-dose combinations. These are justified for a variety of reasons. These include a) increasing therapeutic efficacy, b) lowering adverse drug effects, c) pharmacokinetic advantages, d) lowering pill load, e) lowering individual drug doses, and f) lowering drug resistance development. Objective: A recently approved fixed dose combination of azelnidipine (8 mg) and chlorthalidone (6.25 or 12.5 mg) is indicated to treat hypertension. Individual quantification methods for azelnidipine and chlorthalidone are available, but no practical and acceptable analytical approach for their combination has been documented. As a result, the goal of this literature review was to gather information on numerous analytical instrumental approaches utilized to quantify azelnidipine and chlorthalidone in diverse matrices individually. The scientific community could use this information to design a new analytical method for analysing the recently approved combination. Methods: Authors have explored various scientific databases to obtain information on analytical methods. Results: The methods listed for azelnidipine and chlorthalidone are spectroscopy, highperformance liquid chromatography, hyphenated techniques, high-performance thin-layer chromatography, thin-layer chromatography, and a few other approaches. For azelnidipine and chlorthalidone, there were 26 and 46 research papers reported, respectively.

Background: Genotoxic impurities (GTIs) are produced during the synthesis of active pharmaceutical ingredients and pharmaceutical excipients. L-malic acid, an important active pharmaceutical ingredient and excipient, is widely used in the pharmaceutical industry. However, the detection of potential GTIs in L-malic acid has not been reported. Objective: This study aims to establish a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine the concentration of potential GTIs in L-malic acid, including N-nitroso-aspartic (NASP) and 2-chlorosuccinic acid (CSA). Methods: In this work, GTIs were separated by a reverse-phase Accucore C18 column (100 mm × 2.1 mm, 2.6 μm), with gradient elution using methanol and 0.05% ammonia. The multiple reaction monitoring (MRM) negative mode was used to detect GTIs, with transitional ion pairs of m/z from 131.6 to 88.0 for NASP, and from 150.9 to 70.9 for CSA. Results: The limit of detections (LODs) of NASP and CSA were 2 ng/mL (0.02 ppm) and 5 ng/mL (0.05 ppm), respectively. Both the limit of quantifications (LOQs) of NASP and CSA were 20 ng /mL (0.2 ppm). Good linearity of calibration curves in the concentration ranging from 10 to 500 ng/mL was obtained. The precision was less than 5%, and the intermediate precision was less than 10%. The accuracy ranged from 95.4% to 102.4%, with a relative standard deviation (RSD) of less than 5%. Also, the solution's stability and robustness were acceptable. Conclusion: Compliant with requirements from (International Council for Harmonization) ICH guidelines, this method can be used for routine analysis and stability studies for GTIs’ levels in pharmaceutical quality control.