A systematic and novel quality by design–enabled, rapid, simple, and economic stability–indicating HPLC method for quantifying nirmatrelvir (NMT) was successfully developed and validated. An analytical target profile (ATP) was established, and critical analytical attributes (CAAs) were allocated to meet the ATP requirements. The method used chromatographic separation using a Purosphere column with a 4.6 mm inner diameter × 250 mm (2.5 μm). The analysis occurred at 50°C with a flow rate of 1.2 mL/min and detection at 220 nm. A 10 μL sample was injected, and the mobile phase consisted of two components: mobile phase A, containing 0.1% formic acid in water (20%), and mobile phase B, containing 0.1% formic acid in acetonitrile (80%). The diluent was prepared by mixing acetonitrile and water at a 90:10 v/v ratio. The retention time for the analyte was determined to be 2.78 min. Accuracy exceeded 99%, and the correlation coefficient was greater than 0.999. The validated HPLC method was characterized as precise, accurate, and robust. Significantly, NMT was found to be susceptible to alkaline, acidic, and peroxide conditions during forced degradation testing. The stability-indicating method developed effectively separated the degradation products formed during stress testing, underlining its effectiveness in stability testing and offering accuracy, reliability, and sensitivity in determining NMT. 相似文献
The effect of glass composition and the presence of CdSe/ZnSe nanoparticles (NPs) on the optical absorption and fluorescence of Sm-doped lead borate glasses are studied. Three sets of glass samples xPbO:(99.5-x) B2O3:0.5Sm2O3, x = 29.5–69.5 mol%, xPbO:(96.5-x) B2O3:0.5Sm2O3: 3CdSe/ZnSe, x = 36.5, and 56.5 mol% are prepared. NPs are grown by annealing these glasses just below the glass transition temperature. Average size of both types of NPs increases with annealing time; however, CdSe NPs grew to a larger size range (2 to 20 nm) compared to ZnSe NPs (1 to 16 nm). We analyzed the hypersensitive transition, intensity parameters, radiative transition probability, stimulated emission cross section (σp), and the area ratio of the electric dipole/magnetic dipole transitions of Sm3+. The intensity parameters show a minimum at 11 h annealing for 36.5 mol% and a maximum for the same annealing duration in 56.5 mol% PbO containing CdSe NPs. The σp for 56.5 mol% of PbO with CdSe NPs is found to be a maximum when the average NP size is around 14 nm. ZnSe NPs containing glasses also show significant changes in σp when the average particle size is ~16 nm, for 36.5 mol% PbO. Our results suggest that the optical properties of Sm3+ in lead borate glasses are sensitive to its electronic environment which can be modified by varying the base glass composition and/or incorporating large NPs of CdSe/ZnSe. The large σp values that we observe for some of the glass compositions make them attractive materials for photonic devices and photovoltaic applications.
