The unambiguous quantitation of
racemate involves hydrolysis with 6N D2O/DCl. The amino acids are
derivatized using deuterated reagents. Racemization during this sample
preparation is accompanied by deuterium exchange in the a-position (deuterium
label). The proportion of D-amino acid originally present in the peptide is
thus represent by the relative amounts of the unlabeled form which is
monitored by mass spectrometry.
The limit of quantitation is 0.1% of the optical antipode.
The standard deviation is <0.1%.
What we need:
0.5 to 1mg of the sample (for LOQ of 0.1% of the enantiomer).
The amino acids which are to determine or better the sequence.
Protective groups if present.
Expected content.