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MS TIP No. 5 - Determination of Disulfide Linkages in Biomolecules

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Tip Mass Spec Tips is a collection of tips relating to the operation and service of mass spectrometers. Some of these Tips have been reported in our newsletter, "The Mass Spec Source." If you have a question relating to the operation or service of mass spectrometers or would like to add your comments to the below tip and would like to have it included in this forum, please contact us. Input to this database of MS Tips is needed from our readers to complete this section.

Author: Anonymous

Affiliation: Pharmaceutical Industry

A fast and easy way to detect the presence of disulfide linkages in peptides during static FAB or LISIMS analysis is to dissolve the analyte in a sulfur containing matrix (i.e., thioglycerol, magic bullet, etc.) and add a trace amount of dilute ammonium hydroxide. We have found that this mixture causes immediate reduction of disulfide linkages (converting them to free-SH groups) with the expected 2 dalton mass increase per disulfide group.