Gas chromatographic analysis of amino acid enantiomers in Carbetocin peptide hydrolysates after fast derivatization with pentafluoropropyl chloroformate.
A novel sample preparation protocol for gas chromatographic (GC) analysis of amino acid enantiomers in peptides was developed. It comprises traditional acid hydrolysis, a novel treatment of the analytes with a fluoroalkyl chloroformate and GC/FID separation of enantiomers on a chiral capillary column. The major improvements consist in that the derivatization step proceeds in organic-aqueous media within seconds and the amino acid derivatives are volatile enough to suit the temperature range of the chiral Chirasil-Val capillary column. The approach was found beneficial for chiral analysis of pharmaceutically important Carbetocin peptide.
Zahradnícková
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H
Biology Centre, Academy of Sciences of the Czech Republic, Laboratory of Analytical Biochemistry, Ceské Budejovice, Czech Republic. helenaz@bclab.eu
Hartvich
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P
Simek
P
P
Husek
P
P
D000596:Amino Acids / Q000032:analysis* / Q000138:chemical synthesis; D002138:Calibration; D002849:Chromatography, Gas / Q000379:methods; D005561:Formates / Q000737:chemistry*; D006845:Hydrocarbons, Fluorinated / Q000737:chemistry*; D006868:Hydrolysis; D015394:Molecular Structure; D010121:Oxytocin / Q000031:analogs & derivatives* / Q000737:chemistry; D010446:Peptide Fragments / Q000737:chemistry*; D015203:Reproducibility of Results; D013237:Stereoisomerism; D013997:Time Factors; D005466:Fluorocarbons
D000596:Amino Acids; D005561:Formates; D006845:Hydrocarbons, Fluorinated; D010121:Oxytocin; D010446:Peptide Fragments; C532136:2,2,3,3,3-pentafluoropropyl chloroformate; D005466:Fluorocarbons; C020731:carbetocin