Readily synthesized calibration compounds for quadrupole and magnetic instruments for use over the mass range to 2000 daltons

Volatile mass calibration standards have been prepared by esterifying β‐cellobiose (4‐β‐D‐glucopyranosyl‐D‐glucose) with a mixture of heptafluorobutyric (HFB) anhydride and pentafluoropropionic (PFP) anhydride. The mixed esters produce spectra that are useful for mass spectrometer calibration with positive or negative ion methane chemical ionization and electron impact over the mass range 300–2000. The spectra contain prominent ions spaced at m/z 20 and m/z 50 intervals. Using the mixed ester with direct insertion probe introduction gives intense spectra that persist for tens of minutes. All signals above m/z 194 derived from these substances disappear rapidly upon withdrawal of the probe. The composition and exact masses are given for the positive and negative ion spectra of a mixed HFB/PFP ester of β‐cellobiose. Two other calibrants are described: one made from β‐cellobiose using a mixture of HFB, PFP and trifluoroacetic anhydrides, and another the HFB/PFP mixed ester of perseitol. These are examples of the flexibility of this approach with respect to mass range and ion composition.