title: Critical evaluation of the determination of pharmaceuticals, personal care products, phenolic endocrine disrupters and faecal steroids by GC/MS and PTV-GC/MS in environmental waters.
abstract: An analytical method is described for the determination of a broad range of emerging and priority pollutants, together with sewage molecular markers in environmental waters. The step-by-step study of the GC/MS analyses focuses on the effects of experimental variables using a large volume injection (LVI) technique [a programmed temperature-vaporising (PTV) inlet], the evaluation of a clean-up step using classical and newer sorbents (i.e. Al-N, Fl, NH(2), PSA, Si, CN and DIOL), and the revision of how organic matter [i.e. humic acids (HA) content] affects method performance. Reproducibility and recoveries from spiked coastal water samples at different analyte concentrations (100, 250 and 500 ng L(-1)) as well as with different levels of spiked humic acids (2, 10 and 20 mg L(-1)) are reported indicating a good performance of the extraction procedure with low levels of HA (<10 mg L(-1)). The presence of HA is a critical parameter during the solid-phase extraction (SPE) procedures. Of the clean-up sorbents tested, CN and DIOL proved most efficient in cleaning-up the extracts with recoveries in the range of 66-77% and 100-114%, respectively for the selected analytes. Both GC/MS and PTV-GC/MS instrumental configurations were tested using final sewage effluents, riverine, estuarine and coastal water samples. However, limited applicability of the PTV inlet is reported for environmental applications, affording only a modest improvement in chromatographic signal-to-noise ratios.
authors.affiliation: Plymouth Marine Laboratory, Prospect Place, The Hoe, PL1 3DH, Plymouth, UK. guitart.carlos@gmail.com
authors.forename: Carlos
authors.initials: C
authors.lastname: Guitart
authors.forename: James W
authors.initials: JW
authors.lastname: Readman
mesh_terms: D003358:Cosmetics / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D052244:Endocrine Disruptors / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods; D013256:Steroids / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D003358:Cosmetics; D052244:Endocrine Disruptors; D004364:Pharmaceutical Preparations; D013256:Steroids; D014874:Water Pollutants, Chemical