Abstract

High performance liquid chromatography/mass spectrometry (HPLC/MS) plays an important role in characterizing nonvolatile compounds. There is a strong emphasis for obtaining structural information from HPLC/MS techniques to aid in structural elucidation. Efforts such as immobilized enzyme hydrolysis combined with thermospray HPLC/MS proved useful in characterizing endorphins. Also, the use of chemical derivatization to change proton affinity, volatility or high source temperatures to promote degradation can aid in obtaining structural information for some pharmaceuticals by thermospray HPLC/MS. Most importantly, the combination of particle beam and thermospray HPLC/MS is demonstrated to exhibit the specificity and sensitivity to characterize a wide variety of pharmaceuticals and pesticides. The choice between thermospray or particle beam HPLC/MS method depends on sample volatility, stability and proton affinity. Thermospray provided ample information for the thermally labile and nonvolatile β-lactam antibiotics. Particle beam chemical ionization provided structural information for moderately labile or semi-volatile compounds such as furosemide, spectinomycin, and some pesticides (aldicarb sulfone) and particle beam using electron ionization was useful for more stable and volatile compounds including nitrobenzamides and many pesticides.

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