The novel Vierordt’s approach, or simultaneous equation method, was created and validated for the concurrent determination of vincristine sulfate (VCS) and bovine serum albumin (BSA) in pure solutions utilizing UV spectrophotometry. It is simple, precise, economical, rapid, reliable, and accurate. This method depends on measuring absorbance at two wavelengths, 296 nm and 278 nm, which correspond to the λmax of VCS and BSA in deionized water, respectively. The calibration curves of VCS and BSA are linear at concentration ranges of 10–60 μg/mL and 200–1600 μg/mL, with correlation coefficient values (R2) of 1 and 0.999, respectively. The limits of detection (LOD) and quantification (LOQ) were 0.465 μg/mL and 1.410 μg/mL for VCS and 41.096 μg/mL and 124.533 μg/mL for BSA. The precision investigation indicated that the relative standard deviation (RSD) value was within limitations (RSD < 2%). The percentage recovery varied between 99.40 and 103.20% for VCS and 97.90 and 102.54% for BSA at various concentration levels, demonstrating that the simultaneous equation technique is accurate. The suggested approach can be successfully applied to estimate VCS and BSA simultaneously in pure and pharmaceutical-marketed products comprising these two components.
