Boronate esters are commonly used starting materials in the Suzuki-Miyaura coupling reaction for the C-C bond formation due to their cost-effectiveness and ease of manufacturing process.However, most of them are highly sensitive to moisture and pose challenges during their in-process anal., with conversion to acids under reversed-phase anal. conditions.They are prone to hydrolysis under moisture, pH, and even on-column stationary phases under neutral conditions.At the same time, boronate esters are considered as potential genotoxic substances; hence, their estimation is very important from the patient safety perspective.There are inherent challenges in the existing methods of anal. of these compoundsIn this paper, a convenient, simple, highly sensitive, and greener SFC-MS method was developed for the screening of such unstable boronate esters.The optimized method consisted of Celeris Arginine column (250 mm x 4.6 mm; 5μm) with CO2 (A) as a solvent with a cosolvent of ACN: MeOH (80:20) containing 0.2% 7N methanolic ammonia (B) in gradient mode [Tmin/B %: 0.01/05, 0.50/05, 5.00/50, 7.00/50, 7.10/05, and 10.00/05].Critical method parameters such as ABPR pressure, makeup solvent, additives, and pump flow rate were optimized to enhance the sensitivity with a model compound, i.e., 1-(benzenesulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrrolo[2,3-b]pyridine (CAS number 886547-94-0).The robustness of the method was demonstrated by validating the method as per the ICH guidelines on the same model compound in the concentration range of 0.03-0.3 ppm.The LOD and LOQ for this compound were determined as 0.01 and 0.03 ppm (1 and 3 ppm with respect to API concentrations of 10 mg/mL), resp.The method was successfully applied for the estimation of 16 structurally different boronate esters with no chem. derivatization or hydrolysis.