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Determination of pipecolic acid in serum or plasma by solid-phase extraction and isotope dilution mass spectrometry

1989; Wiley; Volume: 18; Issue: 8 Linguagem: Inglês

10.1002/bms.1200180810

2376-3868

Jan F. Van Bocxlaer, B. J. Verhaeghe, Annick Wauters, W. D. De Marez, Linda M. Thienpont, A.P. De Leenheer,

Analytical Methods in Pharmaceuticals

The determination of pipecolic acid in serum or plasma by positive chemical ionization gas chromatography/mass spectrometry is assessed. This quantitative method involves stable isotope dilution and cation-exchange solid-phase extraction. Several derivatives of pipecolic acid and its octadeuterated analogue were investigated for their mass spectrometric characteristics. The beptafluorobutyric methyl ester derivatives afford optimal resolution on gas chromatography of biological extracts. Moreover, the derivatizing reagent (methanolic HCl) allows a combined elution and derivatization. Selected ion monitoring is performed on the [M + H]+ ions of both analyte and internal standard, at m/z 340 and 348, respectively. Serum or plasma samples from healthy subjects and patients suspected of peroxisomal diseases have been examined.