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The non-conventional Total Ion Current (TIC) detection and corresponding Extracted Ion Current (EIC) chromatogram in LC-MS measurements, have been used for quantitative analysis of reactions involving UV-inactive aza-analogues of deoxycholic acid. LC-(TIC/EIC)-MS experiments allowed for the accurate determination of diastereomeric and overall purity during the development of a new synthetic route for an orthogonally protected dipodal steroid scaffold with defined stereochemistry. Moreover, this technique facilitated adequate monitoring of further scaffold derivatization on solid support. The described methodology offers an attractive solution in cases where conventional HPLC analysis with UV detection fails.

LC-(TIC/EIC)-MS as tool in the analysis of diastereomeric 3,12-aza-analogues of deoxycholic acid