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Clinical Chemistry 47: 2124-2130, 2001;
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(Clinical Chemistry. 2001;47:2124-2130.)
© 2001 American Association for Clinical Chemistry, Inc.

Articles

Determination of L-Pipecolic Acid in Plasma Using Chiral Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Mohamed S. Rashed1a, Lujane Y. Al-Ahaidib1, Hassan Y. Aboul-Enein2, Mohamed Al-Amoudi1 and Minnie Jacob1

1 Metabolic Screening Laboratory and
2 Pharmaceutical Analysis Laboratory, King Faisal Specialist Hospital and Research Centre, MBC-03, PO Box 3354, Riyadh 11211, Saudi Arabia.

aAuthor for correspondence. Fax 966-1-442-4546; e-mail rashed{at}kfshrc.edu.sa.

Background: L-Pipecolic acid (L-PA), an important biochemical marker for the diagnosis of peroxisomal disorders, is usually determined as the racemate. We developed a chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of L-PA in plasma.

Methods: We used a narrow bore chiral macrocyclic glycopeptide teicoplanin column for the enantioseparation of D-pipecolic acid (D-PA) and L-PA and interfaced the column directly to the electrospray source of a tandem mass spectrometer. We used phenylalanine-d5 as internal standard added to 50 µL of plasma followed by deproteinization, evaporation, and injection. The analysis was performed in the selected-reaction monitoring mode using two transitions: m/z 130->m/z 84 for PA, and m/z 171->m/z 125 for phenylalanine-d5. L-PA eluted at 7 min, and D-PA eluted at 11.7 min, whereas phenylalanine-d5 eluted at 6 min. The turnaround time for the assay was 20 min.

Results: Linear calibration curves were obtained in the range of 0.5–80 µmol/L. At a plasma concentration of 1.0 µmol/L, the signal-to-noise ratio was 50:1. The intra- and interassay variations were 3.1–7.9% and 5.7–13%, respectively, at concentrations of 1–50 µmol/L. Mean recoveries of L-PA added to plasma were 95% (5 µmol/L) and 102% (50 µmol/L). The method clearly distinguished between healthy individuals and peroxisomal disease patients.

Conclusions: The novel LC-MS/MS method is simple, rapid, and stereoselective, and uses only 50 µL of plasma, no derivatizing reagents, and a commercially available internal standard. Sample preparation is not complex and is faster than for all other methods.






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