Examples of Analytical Methods
Successfully Adopted
or Developed for Routine Applications:
Using LC and FAB-MS and MS/MS:
1. Generation of tryptic peptide maps of proteins by LC, and structure elucidation / structure confirmation of selected peptides by FAB/MS/MS (e.g., ß-actin in red blood cell membrane, P.I.: Dr. Steven R. Goodman, Cell Biology and Neuroscience).
2. Synthesis and structure confirmation of asymmetric cystine-peptides (P.I.: Dr. Steven Goodman). Method: coupling a cysteine peptide to an arylsulphenyl-activated second one, and verifying the synthesis by FAB / MS and MS/MS.
3. Analysis of N-acetylcysteine in red blood cells (P.I.: Dr. Steven R. Goodman). Method: LC with fluorescence detection of the N-acetylcysteinyl bimane derivative.
Using GC/MS or/and GC/MS/MS with electron ionization:
4. Sex steroid determination in the blood of squirrel monkeys (P.I.: Dr. Christian Abee, Comparative Medicine). Method: EI GC/MS and GC/MS/MS of the heptafluorobutiryl derivatives of testosterone and estradiol.
5. Determination of propyleneglycol in blood of pediatric intensive care patients receiving lorazepam infusion (P.I.: Dr. Michael Chicella, Pediatrics). Method: +EI GC/MS of underivatized propyleneglycol using Supelcowax capillary and 1,2-butanediol as internal standard.
6. Assessing intestinal permeabilities of newborn infants by urinary lactulose / mannitol ratios (P.I.: Dr. Michael Zayek, Pediatrics). Method: +EI GC/MS quantification of the trimethylsilylated lactulose and mannitol.
7. Determination of Capsaicin and its analogues in muscle and plant tissues (P.I.: Dr. Walter Wilborn, Structural Research Center, Mobile, AL). Method: +EI GC/MS of the stabilized trimethylsilyl (TMS) derivative.
8. Elucidation of depolimerization reactions of synthetic rubber polymers in supercritical toluene (P.I.: Dr. Jagdish Dhawan, Chemical Engineering). Method: comparative GC/MS analyses of the products obtained in a micro oven with the toluene and 13C-toluene reagents/solvents.
9. Determination of petrochemical taint components in seafood and in harvest waters (P.I.: Aladar Bencsath, US FDA). Method: dynamic headspace GC/MS.
Using electron capture negative chemical ionization GC/MS:
10. Determination of gamma aminobutyric acid (GABA) in blood plasma (P.I.: Dr. Dirk Dhossche, Psychiatry). Method: electroncapture NCI GC/MS of the perfluoroacyl GABA derivative.
11. Analysis of putrescine in cell extract (P.I.: Dr. Jack Olson, Pharmacology). Method: EC-NCI GC/MS of the heptafluorobutiryl derivative.
12. Determination of chloramphenicol residues
in seafood at picogram levels (P.I.: Dr. Steven Plakas, US FDA). Method:
high resolution EC NCI GC/MS of the trimethylsilyl derivative.