What is the best way to derive D3 and D5 Estradiol for analysis with a Triple Quad and Orbitrab mass spectrometer ?

09 January 2015 1 2K Report

Using Dansyl Chloride to derive samples of D3 Estradiol appeared to work correctly, using a D5 Estradiol sample the derivatization no longer appears to work.

Using an AB Sciex Triple Quadrupole Mass Spectrometer and a Thermo Orbitrap Mass Spectrometer

Kristin Jones

To elaborate, the d5 dansylation reagents were: 50ng d5-Estradiol, 200uL 100mM NaHCO3 (pH=10.5), 100uL 1mg/mL dansyl chloride (in acetonitrile). 20 min at 30C. Q1 infusion showed a massive ion at m/z 251, where 511 was anticipated. 251 doesn't correspond to native, underivatized or derivatized Estradiol, underivatized or derivatized d5-Estradiol, or dansyl chloride. The manufacturer of the d5 suggested differences in ion optics in the QQQ 6500 are producing this 251, but the same product is observed on an Orbitrap Classic. Any thoughts?

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