NEW PERSPECTIVE ON THE DETERMINATION OF FLAME RETARDANTS IN SEWAGE SLUDGE BY USING ULTRAHIGH PRESSURE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY WITH DIFFERENT ION SOURCES

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Abstract

Analysis of 11 polybrominated diphenyl ethers (PBDEs), tetrabromobisphenol A bis 2,3-dibromopropylether (TBBPA-bis), tetrachlorobisphenol A (TCBPA), tetrabromobisphenol A (TBBPA)and hexabromocyclododecanes (HBCDs) was optimized by ultrahigh pressure liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) operating in negative ion (NI) mode. Electrosprayionization (ESI), atmospheric pressure photoionization (APPI) and atmospheric pressure chemicalionization (APCI) sources were tested and for PBDEs APCI gave higher sensitivity than APPI whilefor TBBPA-bis APCI and APPI showed similar performance. ESI was the best option for TCBPA, TBBPAand HBCDs. Detection limits were between 20 and 59 fg for the compounds analyzed by ESI, 0.10and 0.72 pg for PBDEs and 6 pg for TBBPA-bis. The matrix effect of sewage sludge extract was alsotested showing negligible ion suppression for APCI and an increase of the background level of allinvestigated pollutants leading to a worsening of the limits of quantification by a factor between 1.2 and3.3. The UPLC-APCI/MS/MS method for PBDEs, after pressurized liquid extraction (PLE), was validatedby comparison with the concentration values from the NIST 1944 standard reference material. Theadvantages of the methods include low detection limits, PBDE congeners specificity using selectedmultiple reaction monitoring (MRM) transitions, and the absence of thermal degradation of higher PBDEcongeners, especially BDE-209. The methods were applied for the determination of the above reportedflame retardants in sewage sludge in order to get more information about the degradation on PBDEs(in particular BDE-209) during municipal wastewater treatments.

Autore Pugliese

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  • MASCOLO G.; LOCAPUTO V.; MININNI G.

Titolo volume/Rivista

Journal of chromatography

Anno di pubblicazione

2010

ISSN

0021-9673

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