Document Detail


Determination of musk fragrances in sewage sludge by pressurized liquid extraction coupled to automated ionic liquid-based headspace single-drop microextraction followed by GC-MS/MS.
MedLine Citation:
PMID:  23019133     Owner:  NLM     Status:  Publisher    
Abstract/OtherAbstract:
A method for the quantitative determination of ten musk fragrances extensively used in personal care products from sewage sludge was developed by using a pressurized liquid extraction (PLE) followed by an automated ionic liquid-based headspace single-drop microextraction and gas chromatography-tandem mass spectrometry. The influence of main factors on the efficiency of PLE was studied. For all musks, the highest recovery values were achieved using 1 g of pretreated sewage sludge, H(2) O/methanol (1:1) as an extraction solvent, a temperature of 80°C, a pressure of 1500 psi, an extraction time of 5 min, 2 cycles, a 100% flush volume, a purge time of 120 s, and 1 g Florisil as in-cell clean-up extraction sorbent. The use and optimization of an in-cell clean-up sorbent was necessary to remove fatty interferents of the PLE extract that make the subsequent ionic liquid-based headspace single-drop microextraction difficult. Validation parameters, namely LODs and LOQs, ranged from 0.5-1.5 to 2.5-5 ng/g, respectively. Good levels of intra- and interday repeatabilities were obtained analyzing sewage sludge samples spiked at 10 ng/g (n = 3, RSDs < 10%). The method applicability was tested with sewage sludge from different wastewater treatment plants. The analysis revealed the presence of all the polycyclic musks studied at concentrations higher than the LOQs, ranging from 6 to 530 ng/g. However, the nitro musk concentrations were below the LOQs or, in the case of musk xylene, was not detected.
Authors:
Laura Vallecillos; Francesc Borrull; Eva Pocurull
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2012-9-28
Journal Detail:
Title:  Journal of separation science     Volume:  -     ISSN:  1615-9314     ISO Abbreviation:  J Sep Sci     Publication Date:  2012 Sep 
Date Detail:
Created Date:  2012-9-28     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101088554     Medline TA:  J Sep Sci     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
Copyright Information:
© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Affiliation:
Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Tarragona, Spain.
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