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The MS/MS spectra of peak 3 from the peptide reacted in D 2 O showed that all of the fragment ions containing residue 103 (isoAsp103) (y 9 , y 10 , y 11 , y 12 , b 13 , and b 14 2+ ) were shifted by 1 Da compared to the corresponding fragment ions from the peptide reacted in H 2 O, unequivocally indicating that residue 103 was the site of deuterium incorporation and, thus, the location of isoAsp