PMID- 19201001
OWN - NLM
STAT- MEDLINE
DCOM- 20090813
LR  - 20131121
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1216
IP  - 12
DP  - 2009 Mar 20
TI  - Multiresidue analysis of pollutants as their trimethylsilyl derivatives, by gas 
      chromatography-mass spectrometry.
PG  - 2288-301
LID - 10.1016/j.chroma.2009.01.056 [doi]
AB  - This paper reports a multiresidue analysis procedure which permits the 
      identification and quantification of sixty-three water-soluble pollutants. 
      Subsequent to their solid-phase extraction (SPE) enrichment, analyses of species 
      have been carried out from one solution, by a single injection, as their 
      trimethylsilyl-oxime ether/ester derivatives, by gas chromatography-mass 
      spectrometry, within 31min. Based on our optimized extraction, derivatization and 
      mass fragmentation studies separation have been performed in the total ion 
      current mode, identification and quantification of compounds have been carried 
      out on the basis of their selective fragment ions. Including various 
      pharmaceuticals, benzoic acid, its substituted species, different aromatic 
      carboxylic acids, cholic acids, unsaturated and saturated fatty acids, aliphatic 
      dicarboxylic acids, as well as synthetic pollutants of various origins 
      (2,4-di-tert-butylphenol, different phthalates). Standard compounds were added to 
      500 mL effluent wastewater samples, at three concentrations (1-5 microg/L, 5-10 
      microg/L and 10-20 microg/L). Recoveries, using the Waters Oasis cartridges 
      performing extractions at pH 2, pH 4 and pH 7 proved to be the optimum at pH 4 
      (average recoveries (94.5%), except for cholesterol (10%), paracetamol (18%) and 
      2,5-dihydroxybenzoic acid (25%). Carbamazepine could be recovered at pH 7, only. 
      Responses, obtained with derivatized standards proved to be linear in the range 
      of 4-80 microg/L levels. Limit of quantitation values varied between 0.92 ng/L 
      (4-hydroxyphenylacetic acid) and 600 ng/L (dehydrocholic acid) concentrations. 
      One of the most important messages of this work is the confirmation of the origin 
      of blank values. It was shown that contaminants, mainly 2,4-di-tert-butylphenol, 
      different phthalates and fatty acids, are sourced both from the reagents and 
      mainly from the SPE procedure, independent on the cartridge applied. 
      Reproducibilities, characterized with the relative standard deviations (RSDs) of 
      measurements, varied between 0.71% and 10%, with an average of 4.38% RSD. The 
      practical utility of the method was shown by the identification and 
      quantification of the pollutant contents of Hungarian influent and effluent 
      wastewaters (for six consecutive months and that of the Danube River for 2 
      months).
FAU - Sebok, A
AU  - Sebok A
AD  - Department of Analytical Chemistry, Institute of Chemistry, L Eotvos University, 
      Budapest, Hungary.
FAU - Vasanits-Zsigrai, A
AU  - Vasanits-Zsigrai A
FAU - Helenkar, A
AU  - Helenkar A
FAU - Zaray, Gy
AU  - Zaray G
FAU - Molnar-Perl, I
AU  - Molnar-Perl I
LA  - eng
PT  - Journal Article
DEP - 20090123
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Benzhydryl Compounds)
RN  - 0 (Phenols)
RN  - 0 (Phthalic Acids)
RN  - 0 (Sewage)
RN  - 0 (Trimethylsilyl Compounds)
RN  - 0 (Water Pollutants, Chemical)
RN  - MLT3645I99 (bisphenol A)
SB  - IM
MH  - Benzhydryl Compounds
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Hydrogen-Ion Concentration
MH  - Models, Chemical
MH  - Phenols/analysis
MH  - Phthalic Acids/analysis
MH  - Reproducibility of Results
MH  - Research Design
MH  - Rivers/chemistry
MH  - Sensitivity and Specificity
MH  - Sewage/chemistry
MH  - Solid Phase Extraction/*methods
MH  - Trimethylsilyl Compounds/analysis/*chemical synthesis
MH  - Water Pollutants, Chemical/*analysis
EDAT- 2009/02/10 09:00
MHDA- 2009/08/14 09:00
CRDT- 2009/02/10 09:00
PHST- 2008/10/14 00:00 [received]
PHST- 2009/01/16 00:00 [revised]
PHST- 2009/01/19 00:00 [accepted]
PHST- 2009/02/10 09:00 [entrez]
PHST- 2009/02/10 09:00 [pubmed]
PHST- 2009/08/14 09:00 [medline]
AID - S0021-9673(09)00119-8 [pii]
AID - 10.1016/j.chroma.2009.01.056 [doi]
PST - ppublish
SO  - J Chromatogr A. 2009 Mar 20;1216(12):2288-301. doi: 10.1016/j.chroma.2009.01.056. 
      Epub 2009 Jan 23.