title: Solid phase analytical derivatization of anthropogenic and natural phenolic estrogen mimics with pentafluoropyridine for gas chromatography-mass spectrometry.
abstract: A simple, low cost, fast and sensitive method is reported for the determination of the four endocrine disrupting chemicals (EDCs) 4-tert-butylphenol, 4-tert-octylphenol, bisphenol A and 17β-estradiol using pentafluoropyridine as the derivatizing reagent. These EDCs were determined by simultaneous extraction and derivatization in a solid phase analytical derivatization (SPAD) technique without the aid of any phase transfer catalyst (PTC) or an ion-pair mechanism. Recoveries of analytes as their tetrafluoropyridyl derivatives from water ranged from 71% for 4-tert-butylphenol to 106% for 17β-estradiol; from urine they ranged from 61% for 17β-estradiol to 91% for 4-tert-octylphenol; and from humic acids solution the ranged from 59% for 17β-estradiol to 104% for 4-tert-octylphenol in humic acid solutions. Calibration curves were constructed from a matrix of human male urine in the range 1-40 ng/mL and had coefficients of correlation greater than 0.99. For 4-tert-butylphenol, bisphenol A and 17β-estradiol the limits of quantitation were 5 ng/mL and for 4-tert-octylphenol it was 1 ng/mL. This method was applied to determine EDCs and detected 4-tert-octylphenol, bisphenol A and 17β-estradiol in concentrations comparable to those found in the literature. The method offers advantages in speed of analysis, reduced reagent and specificity of derivatization.
authors: Department of Pathology and Molecular Medicine, McMaster University Medical Centre 3N26 1200 Main St. W. Hamilton On. L8N 3Z5, Canada.
authors: Sanka N
authors: SN
authors: Atapattu
authors: Jack M
authors: JM
authors: Rosenfeld
mesh_terms: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors / Q000032:analysis* / Q000652:urine; D004958:Estradiol / Q000032:analysis* / Q000652:urine; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006812:Humic Substances / Q000032:analysis; D008297:Male; D010636:Phenols / Q000032:analysis* / Q000652:urine; D011725:Pyridines / Q000737:chemistry; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D014867:Water / Q000737:chemistry; D005466:Fluorocarbons; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors; D004958:Estradiol; D006812:Humic Substances; D010636:Phenols; D011725:Pyridines; D014867:Water; C486857:pentafluoropyridine; D005466:Fluorocarbons; C105260:4-tert-octylphenol; C006780:bisphenol A; D000098826:Bisphenol A Compounds; C006862:butylphen