A method for the selective determination of formaldehyde and acetaldehyde in air samples based on HPLC-APCI-MS with calibration using stable isotope-labelled standards was developed. d2-Formaldehyde-2,4-dinitrophenylhydrazone and d4-acetaldehyde-2,4-dinitrophenylhydrazone were synthesized from 2,4-dinitrophenylhydrazine and the respective deuterated aldehydes. The labelled derivatives were used as internal calibration standards in the quantification of formaldehyde and acetaldehyde in complex matrices, including automobile exhaust. Co-elution of the labelled and non-labelled derivatives in HPLC provides for identical mass spectrometric conditions, thus significantly reducing the relative standard deviation of the internal calibration approach compared with external calibration with non-labelled derivatives.
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Zurek et al. (1999) studied this question.
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