Separations

Mixed amine/sulfolane (TMS) biphasic solutions have gained attention for their adjustable structure–activity relationships and lower regeneration energy. In this study, monoethanolamine (MEA) is employed as the main absorbent and polyamine as the co-absorbent, which are subsequently mixed with the phase separation promoter sulfolane (TMS) to form ternary biphasic solvent systems. Polyamine co-absorbents include 3-Dimethylaminopropylamine (DMAPA), 3-Diethylaminopropylamine (DEAPA), and Diethylenetriamine (DETA). Phase separation, absorption, and desorption performances were systematically studied. Reaction and phase separation mechanisms were elucidated through ¹³C nuclear magnetic resonance (NMR) spectroscopy. The overall mass transfer coefficients (K_G) were measured using a wetted wall column (WWC). Variations in the amine-to-sulfolane concentration ratio showed minimal impact on phase volume, while temperature and solvent composition significantly influenced phase separation behavior. All three solvents exhibited superior CO₂ capture performance, with CO₂ loadings in the rich phases ranging from 4.09 to 4.71 mol/L and over 96.82% of CO₂ concentrated in them, cyclic capacities reached or exceeded 3 mol/L, and regeneration energy consumption was 29.63–55.51% lower than 5 M MEA. ¹³C NMR analysis indicated that multiple N atoms in polyamines promoted the formation of additional ionic species during CO₂ absorption, thereby enhancing phase separation completeness. Furthermore, K_G values for the ternary systems exceeded that of conventional MEA, with the MEA/DEAPA/TMS system exhibiting a 1.7-fold increase. These findings demonstrated the industrial potential of MEA/polyamine/TMS biphasic solvents for efficient CO₂ capture.

Over the past few years, the misuse of medications has progressively increased, posing a significant public health concern. This study proposed the development and validation of an alternative and greener analytical method for the determination of dextromethorphan (DXM) and its major metabolite, dextrorphan (DXO), in urine matrices using bar adsorptive microextraction (BAμE), followed by gas chromatography–mass spectrometry (GC-MS) analysis. Under optimized experimental conditions, average recoveries of 96.3% and 80.4% were achieved for DXM and DXO, respectively. The analytical limits obtained were 0.016 μg/mL for the limit of detection and 0.054 μg/mL for the limit of quantification. The working range was from 0.06 μg/mL to 2.0 μg/mL, with linearity for both compounds by determination coefficients (r² > 0.99) and the goodness-of-fit and lack-of-fit tests. Intra-day precision and trueness yielded values below 8.77% and 16.28%, respectively, for both compounds. Inter-day precision and trueness values were below 7.67% and 9.73%, respectively. The application to 26 urine samples allowed the quantification of both compounds, with concentrations ranging from 0.06 to 3.21 μg/mL for DXM and 0.06 to 8.88 μg/mL for DXO. The method proved to be effective, selective, sensitive, simple, and cost-effective in the detection and quantification of DXM and DXO, reinforcing its applicability and feasibility in various laboratory contexts.

A robust and stability-indicating Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the quantitative determination of bexagliflozin and its related impurities in accordance with the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH Q2(R1)) guidelines. Chromatographic separation was achieved on a C18 column using a mobile phase of methanol and ammonium acetate buffer (pH 4.2) in a 60:40 (v/v) ratio, with a flow rate of 1.0 mL·min⁻¹ and UV detection at 220 nm. The method was validated for linearity, sensitivity (LOD and LOQ), precision, robustness, and system suitability, all within acceptable limits for low-concentration analysis. Excellent linearity (r² > 0.999) and precision (%RSD 0.3–4.4%) confirmed its reliability for stability assessment. The assay was performed at 100 µg·mL⁻¹, where all validation parameters showed %RSD values ≤ 2%, demonstrating high precision and robustness. Forced degradation studies under acidic, basic, oxidative, photolytic, and thermal conditions revealed a major degradation product formed under acidic stress. This product was isolated and structurally characterized using LC–MS, ¹H NMR, and ¹³C NMR, and is reported here for the first time. The proposed RP-HPLC method proved to be specific, precise, and reliable for the determination of bexagliflozin and its related impurities, making it suitable for routine stability testing, quality control, and pharmaceutical development applications.