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Medroxyprogesterone acetate (MPA) is one of the major drugs used in endocrine therapy for advanced or recurrent breast cancer. The present study describes an accurate and reproducible gas chromatographic-mass spectrometric (GC-MS) method to measure MPA in serum. After being extracted by a solid-phase cartridge using an Oasis HLB copolymer, the residues were derivatized with a heptafluorobutyric anhydride and then analyzed by GC-MS.

We validated the method by analyzing the serum samples spiked with pure MPA, and obtained a linear correlation (0.9977) and precision with a coefficient of variation ranging from 1.8 to 73. We found that the GC-MS method was linear over the range of 0.2 ng mL(-1) to 500 ng mL(-1) using a sample volume of 1 mL The analytical recovery was 93.7%, and the limit of detection was 0.2 ng mL(-1).

The oral administration of MPA to men and its subsequent detection in serum showed that the GC-MS method described is sensitive, specific, and suitable for the determination of MPA by bench-top GC-MS.