Monolithic packed 96-tips set for high-throughput sample preparation: determination of cyclophosphamide and busulfan in whole blood samples by monolithic packed 96-tips and LC-MS.

A monolithic methacrylate packed 96-tips device was used for the extraction of the busulfan and cyclophosphamide in whole blood samples. Using a packed 96-tips set, a 96-well plate could be handled in about 2 min. The key aspect of the monolithic phase is that monolithic material can offer both good extraction capacity and low-back-pressure properties. The validation of the methodology showed that the accuracy values of quality-control samples were between 99 and 113% for busulfan, and between 103 and 110% for cyclophosphamide. The inter-day precision ranged from 7.0 to 12% for busulfan and from 13 to 16% for cyclophosphamide. The standard calibration curves were obtained within the concentration range 5-2000 nm for busulfan and from 10 to 5000 nm for cyclophosphamide in blood samples. The coefficients of determination were ≥0.99.