Orthogonal extraction/chromatography and UPLC, two powerful new techniques for bioanalytical quantitation of desloratadine and 3-hydroxydesloratadine at 25 pg/mL.

ABSTRACT

Validation of the bioanalytical method for determination of desloratadine and 3-hydroxydesloratadine was conducted using ultra high pressure liquid chromatography (UPLC) in conjunction with mix mode solid phase extraction. The dynamic range of the assay was from 0.025 ng/mL to 10 ng/mL using 96-well solid phase extraction. On an UPLC system, the inter-run accuracy was better than 94.7% for desloratadine (n = 18) and 94.0% for 3-hydroxydesloratadine (n = 18). The between-run precision (%CV) ranged from 2.6% to 9.8% for desloratadine (n = 18) and 3.1% to 11.1% for 3-hydroxydesloratadine (n = 18). The limit of quantitation represented 0.478 pg and 0.525 pg of extracted material injected on-column for desloratadine and 3-hydroxydesloratadine, respectively. The total run time was slightly over 2 min per sample. The approach of orthogonal extraction/chromatography and UPLC significantly improves assay performance while also increasing sample throughput for drug development studies.