Determination of ortho-phenylphenol in human urine by gas chromatography-mass spectrometry.
A sensitive gas chromatographic-mass spectrometric method was developed to quantitate total o-phenylphenol (OPP) (free plus conjugates) in human urine. Conjugates of OPP were acid-hydrolyzed to free OPP, derivatized to the pentafluorobenzoyl ester derivative and analyzed via negative-ion chemical ionization gas chromatography-mass spectrometry. Two stable isotope analogs of OPP were shown to be suitable as internal standards for this method (D2-phenol ring, 13C6-phenyl ring). A synthetic method is presented for the preparation of the D2-OPP internal standard. The 13C6-OPP analog was also shown to be useful as an alternate test material for laboratory-based exposure studies. The limit of quantitation for this method was 1 ng OPP/ml urine. Calibration curves were linear for the analyte over the concentration range of 0.5-1117 ng OPP/ml urine. Relative recovery of OPP from urine ranged from 97.0 to 104.7%. Low levels of OPP (mean=6+/-7 ng/ml; n=22) were found in control human urine samples. The method was validated with urine samples obtained from human volunteers undergoing a dermal exposure study with 12C-/13C6-/14C-OPP. This method was developed to aid in assessments of human exposure to OPP during a variety of uses of the compound.
Bartels
M J
MJ
Health and Environmental Research Laboratories, The Dow Chemical Company, Midland, MI 48674, USA.
Brzak
K A
KA
Bormett
G A
GA
D001713:Biphenyl Compounds / Q000032:analysis / Q000737:chemistry / Q000652:urine*; D002247:Carbon Isotopes; D002940:Circadian Rhythm; D003903:Deuterium; D005659:Fungicides, Industrial / Q000032:analysis / Q000737:chemistry / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D016014:Linear Models; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D001713:Biphenyl Compounds; D002247:Carbon Isotopes; D005659:Fungicides, Industrial; D003903:Deuterium; C004369:2-phenylphenol