Identification and quantitative determination of m-hydroxyphenylglycol in mammalian urine.

m-Hydroxyphenylglycol (MHPG) has been identified in mammalian urine by gas chromatography mass spectrometry selected ion monitoring. (2H0) MHPG and (2H5) MHPG were synthesized for use as authentic sample and internal standard, respectively. After acid hydrolysis or treatment with sulfatase, the glycol was extracted from urine with ethyl acetate, converted to its tris-pentafluoropropionyl (PFP) derivative and identified by comparison of the retention times and relative intensities of the characteristic ions, m/z 592, m/z 428 and m/z 415, with those from the authentic sample. Using the internal standard the following quantitative results were obtained: 10 normal human adults excreted 7 ng MHPG mg-1 creatinine (range 2-18) as a sulfate conjugate. Ten rats excreted 0.8 micrograms day-1 (range 0.5-1.1) of MHPG also in the conjugated form. Urinary m-hydroxymandelic acid (MHMA) was also measured quantitatively. The ratio MHMA:MHPG was 1:1 in the rat and 6:1 in the human. This indicates that the overall reductive pathway of m-octopamine and m-synephrine metabolism is more important in the rat than in the human. o-Hydroxyphenylglycol (OHPG) and the three isomeric monomethoxy phenylglycols could not be detected in human or rat urine by these techniques.