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This study represents a comparison among the performances of four multivariate procedures: partial least square (PLS) and artificial neural networks (ANN) in addition to support vector regression (SVR) and extreme gradient boosting (XG Boost) algorithm for the determination of the anti-diabetic mixture of pioglitazone (PIO), alogliptin (ALG) and glimepiride (GLM) in pharmaceutical formulations with aid of UV spectrometry. Key wavelengths were selected using knowledge-based variable selection and various preprocessing methods (e.g., mean centering, orthogonal scatter correction, and principal component analysis) to minimize noise and improve model precision. XG Boost effectively enhanced computing speed and accuracy by focusing on specific spectral features rather than the entire spectrum, demonstrating its advantages in resolving complex, overlapping spectral data. The independent test results of different models demonstrated that XG Boost outperformed other methods. XG Boost achieved the lowest root mean squared error of prediction (RMSEP) and standard deviation (SD) values across all compounds, indicating minimal prediction error and variability. For PIO, XG Boost recorded an RMSEP of 0.100 and SD of 0.369, significantly better than PLS and ANN. For ALG, XG Boost showed near-perfect performance with an RMSEP of 0.001 and SD of 0.005, outperforming SVR and PLS, which had higher error rates. In the case of GLM, XG Boost also excelled with an RMSEP of 0.001 and SD of 0.018, demonstrating superior precision compared to the much higher errors seen in PLS and ANN. These results highlight XG Boost's exceptional ability to handle complex, overlapping spectral data, making it the most reliable and accurate model in this study. [ABSTRACT FROM AUTHOR]

In this study, bupivacaine (BUP) and meloxicam (MLX) were simultaneously assayed in their co-formulated ampoules without interference using four affordable, sensitive, and eco-friendly spectrophotometric methods. The assay of MLX at 359.3 nm over the concentration range of 1.0–15.0 µg/mL was accomplished using a direct UV-spectrophotometric method (Method I) without interference from BUP. However, there was a significant overlap between the spectra of BUP and MLX, making it difficult to determine BUP directly from the UV spectrum. Therefore, various UV-based techniques, including second derivative spectrophotometry (Method II), ratio subtraction method (Method III), and absorption factor method (Method IV), were used to determine BUP over the concentration range of 5.0–80.0 µg/mL. The proposed methods could simultaneously determine the studied drugs with a challenging ratio of 33.3:1.0 (BUP: MLX), which increases the importance of the current study. The proposed methods were applied to estimate the studied drugs in commercial ampoules with high % recoveries and low %RSD values. The excellent eco-friendliness of the developed methods was demonstrated using GAPI and AGREE metrics. The developed methods were validated according to ICHQ2(R2) guidelines. The proposed methods can be better suited for the routine analysis of BUP and MLX in their fixed-dose combination with high selectivity. [ABSTRACT FROM AUTHOR]

Food and Drug Administration (FDA) recently approved co-formulated celecoxib and tramadol for the treatment of acute pain in adults. Three spectrophotometric methods were efficiently applied to estimate the co-formulated Celecoxib and Tramadol in their tablets; second derivative 2D-spectrophotometry technique (method I), induced dual-wavelength technique (method II) and dual-wavelength resolution technique (method III). The proposed methods were successfully validated following the International Council for Harmonisation (ICH) guidelines and statistically assessed based on the correlation coefficients, relative standard deviations as well as detection and quantitation limits. The obtained results revealed non-significant differences compared to the reported results as revealed by the variance ratio F test and Student t test. Moreover, the applied techniques were further assessed concerning their greenness based on the analytical eco-scale method revealing an excellent green scale with a final score of 95. The proposed spectrophotometric techniques could be applied for the routine analysis and quality control of the studied drugs in their dosage form. [ABSTRACT FROM AUTHOR]

A reversed-phase RP-HPLC method was developed for the simultaneous determination of metformin hydrochloride (MET), pioglitazone (PIO), and glimepiride (GLM) in their combined dosage forms and spiked human plasma. Quality risk management principles for determining the critical method parameters (CMPs) and fractional factorial design were made to screen CMPs and subsequently, the Box–Behnken design was employed. The analytical Quality by Design (AQbD) paradigm was used to establish the method operable design region (MODR) for the developed method depended on understanding the quality target product profile (QTPP), analytical target profile (ATP), and risk assessment for different factors that affect the method performance to develop an accurate, precise, cost-effective, and environmentally benign method. The separation was carried out using a mobile phase composed of methanol: 0.05 M potassium dihydrogen phosphate buffer pH 3.7 with 0.05% TEA (78:22, v/v). The flow rate was 1.2 mL/min. DAD detector was set at 227 nm. Linagliptin (LIN) was used as an internal standard. The proposed method was validated according to The International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The assay results obtained by using the developed method were statistically compared to those obtained by the reported HPLC method, and a satisfying agreement was observed. [ABSTRACT FROM AUTHOR]

Telmisartan (TEL) and Nebivolol (NEB) are frequently co-formulated in a single dosage form that is frequently prescribed for the treatment of hypertension, moreover, telmisartan is currently proposed to be used to treat COVID19-induced lung inflammation. Green rapid, simple, and sensitive synchronous spectrofluorimetric techniques for simultaneous estimation of TEL and NEB in their co-formulated pharmaceutical preparations and human plasma were developed and validated. Synchronous fluorescence intensity at 335 nm was used for TEL determination (Method I). For the mixture, the first derivative synchronous peak amplitudes (D1) at 296.3 and 320.5 nm were used for simultaneous estimation of NEB and TEL, respectively (Method II). The calibration plots were rectilinear over the concentration ranges of 30–550 ng/mL, and 50–800 ng/mL for NEB and TEL, respectively. The high sensitivity of the developed methods allowed for their analysis in human plasma samples. NEB's Quantum yield was estimated by applying the single-point method. The greenness of the proposed approaches was evaluated using the Eco-scale, National Environmental Method Index (NEMI), and Green Analytical Procedure Index (GAPI) methods. [ABSTRACT FROM AUTHOR]

A simple and sensitive voltammetric method was developed and validated for the recognition of the veterinary drug nitroxynil (NTX). The method is based on studying its voltammetric behavior at a carbon paste electrode. Square wave voltammetry (SWV) was successfully applied in this study. The anodic peak current obtained was a linear function of NTX concentration in Britton Robinson buffer of pH 3 over the range of 3.9 × 10–6–1.0 × 10−4 M with lower detection and quantitation limits of 3.1 × 10–7 and 9.4 × 10–7 M, respectively. The proposed method was first applied to the assessment of the drug in commercial vials. The method was further used to monitor the residual amounts of the drug in bovine meat, kidney, fat, and milk samples. The results obtained were favourably compared with those given by reference method. The interference likely to be introduced by co-administered drugs was evaluated. The electrode reaction was elucidated, and electron transfer kinetics were studied. [ABSTRACT FROM AUTHOR]