LC/MS is now considered to be the most promising analytical method for
the determination of biological substances, especially nonvolatile or
high molecular weight substances. But one of the drawbacks of this me
thod is its low sensitivity in comparison with GC/MS. In order to over
come this problem, the derivatization methods are used in LC/MS. This
report overviews the detection-oriented derivatization methods in LC/
MS including our results. The typical examples are as follows. The der
ivatization of vitamin D with a Cookson-type reagent (analog of 4-phen
yl-1,2,4-triazoline-3,5-dione) gave satisfactory sensitivity, which wa
s also observed on the derivatization of oxosteroids with O-methylhydr
oxylamine. Although the oxosteroid fatty acid esters gave a de-esterif
ied ion as a base peak in atmospheric pressure chemical-ionization MS,
the methyloxime of which gave a quasimolecular ion as a base peak, wh
ich is helpful to identify the compounds in the brain.