DETERMINATION OF ORTHO-PHENYLPHENOL IN HUMAN URINE BY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

A sensitive gas chromatographic-mass spectrometric method was develope d to quantitate total o-phenylphenol (OPP) (free plus conjugates) in h uman urine. Conjugates of OPP were acid-hydrolyzed to free OPP, deriva tized to the pentafluorobenzoyl ester derivative and analyzed via nega tive-ion chemical ionization gas chromatography-mass spectrometry. Two stable isotope analogs of OPP were shown to be suitable as internal s tandards for this method (D-2-phenol ring, C-13(6)-phenyl ring). A syn thetic method is presented for the preparation of the D-2-OPP internal standard. The C-13(6)-OPP analog was also shown to be useful as an al ternate test material for laboratory-based exposure studies. The limit of quantitation for this method was 1 ng OPP/ml urine. Calibration cu rves were Linear for the analyte over the concentration range of 0.5-1 117 ng OPP/ml urine. Relative recovery of OPP from urine ranged from 9 7.0 to 104.7%. Low levels of OPP (mean = 6 +/- 7 ng/ml; n = 22) were f ound in control human urine samples. The method was validated with uri ne samples obtained from human volunteers undergoing a dermal exposure study with C-12-/C-13(6)-/C-14-OPP. This method was developed to aid in assessments of human exposure to OPP during a variety of uses of th e compound. Published by Elsevier Science B.V.