Analysis of pipecolic acid in biological fluids using capillary gas chromatography with electron-capture detection and [2H11]pipecolic acid as internal standard.

Abstract

A sensitive and accurate stable isotope dilution assay was developed for the measurement of pipecolic acid in body fluids using capillary gas chromatography with electron-capture detection. The method utilizes [2H11]pipecolic acid as the internal standard. Sample preparation consisted of derivatization in aqueous solution (pH 11.5) of the amine moiety with methyl chloroformate to the N-methylcarbamate, followed by acidic ethyl acetate extraction at pH less than or equal to 2 and further derivatization of the carboxyl moiety with pentafluorobenzyl bromide, the excess of which was removed by solid-phase extraction. Control values have been determined in the plasma of at-term infants, age greater than 1 week (n = 21, mean = 1.36 microM, range = 0.47-3.27 microM). The utility of the method was demonstrated by quantitating pipecolic acid in biological fluids derived from patients with peroxisomal disorders. The method was validated against an established electron-capture negative ion mass fragmentographic technique.

• Authors: T Zee, F Stellaard, C Jakobs
• Journal: Journal of chromatography (J Chromatogr) Vol. 574 Issue 2 Pg. 335-9 (Feb 14 1992) Netherlands
• PMID: 1618968 (Publication Type: Journal Article)

Chemical References

• Pipecolic Acids
• pipecolic acid

Topics

• Body Fluids (chemistry)
• Chromatography, Gas
• Electrons
• Humans
• Metabolism, Inborn Errors (blood, cerebrospinal fluid, diagnosis, urine)
• Microbodies (metabolism)
• Pipecolic Acids (blood, cerebrospinal fluid, metabolism, urine)
• Reference Standards