Highly Sensitive and Specific LC-APPI-MS/MS Determination of Ciclesonide and Desciclesonide (M1) in Human Serum (LLOQ: 1 pg/mL)

摘要

A highly sensitive and selective LC-APPI-MS/MS method, with an LLOQ of 1 pg/mL, has been successfully developed for the determination of ciclesonide and M1 in human serum. The method has been fully validated using both 0.5-mL and 0.25-mL serum, following the FDA guidance for Bioanalytical Method Validation. Serum samples are stable for 3 freeze/thaw cycles, or 24 hr ambient, or 1-year frozen storage at both -20°C and -70°C. The method robustness was demonstrated by the successful analysis of thousands of study samples without a single failure and the acceptable incurred sample reproducibility (ISR) testing performance. It was demonstrated that APPI has much better selectivity than ESI for this study.