| Title | NEW PERSPECTIVE ON THE DETERMINATION OF FLAME RETARDANTS IN SEWAGE SLUDGE BY USING ULTRAHIGH PRESSURE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY WITH DIFFERENT ION SOURCES |
| 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. Electrospray
ionization (ESI), atmospheric pressure photoionization (APPI) and atmospheric pressure chemical
ionization (APCI) sources were tested and for PBDEs APCI gave higher sensitivity than APPI while
for TBBPA-bis APCI and APPI showed similar performance. ESI was the best option for TCBPA, TBBPA
and HBCDs. Detection limits were between 20 and 59 fg for the compounds analyzed by ESI, 0.10
and 0.72 pg for PBDEs and 6 pg for TBBPA-bis. The matrix effect of sewage sludge extract was also
tested showing negligible ion suppression for APCI and an increase of the background level of all
investigated pollutants leading to a worsening of the limits of quantification by a factor between 1.2 and
3.3. The UPLC-APCI/MS/MS method for PBDEs, after pressurized liquid extraction (PLE), was validated
by comparison with the concentration values from the NIST 1944 standard reference material. The
advantages of the methods include low detection limits, PBDE congeners specificity using selected
multiple reaction monitoring (MRM) transitions, and the absence of thermal degradation of higher PBDE
congeners, especially BDE-209. The methods were applied for the determination of the above reported
flame retardants in sewage sludge in order to get more information about the degradation on PBDEs
(in particular BDE-209) during municipal wastewater treatments. |
| Source | Journal of chromatography (Print) 1217, pp. 4601–4611 |
| Journal | Journal of chromatography (Print) |
| Editor | Elsevier, Amsterdam, Paesi Bassi |
| Year | 2010 |
| Type | Articolo in rivista |
| DOI | 10.1016/j.chroma.2010.05.003 |
| Authors | MASCOLO G., LOCAPUTO V., MININNI G. |
| Text | 42381 2010 10.1016/j.chroma.2010.05.003 NEW PERSPECTIVE ON THE DETERMINATION OF FLAME RETARDANTS IN SEWAGE SLUDGE BY USING ULTRAHIGH PRESSURE LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY WITH DIFFERENT ION SOURCES MASCOLO G., LOCAPUTO V., MININNI G. a Istituto di Ricerca Sulle Acque, Consiglio Nazionale delle Ricerche, Via F. De Blasio 5, 70123 Bari, Italy b Istituto di Ricerca Sulle Acque, Consiglio Nazionale delle Ricerche, via Salaria km 29, 3, P.O. Box, 10 00016 Monterotondo Rome , Italy 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. Electrospray ionization ESI , atmospheric pressure photoionization APPI and atmospheric pressure chemical ionization APCI sources were tested and for PBDEs APCI gave higher sensitivity than APPI while for TBBPA bis APCI and APPI showed similar performance. ESI was the best option for TCBPA, TBBPA and HBCDs. Detection limits were between 20 and 59 fg for the compounds analyzed by ESI, 0.10 and 0.72 pg for PBDEs and 6 pg for TBBPA bis. The matrix effect of sewage sludge extract was also tested showing negligible ion suppression for APCI and an increase of the background level of all investigated pollutants leading to a worsening of the limits of quantification by a factor between 1.2 and 3.3. The UPLC APCI/MS/MS method for PBDEs, after pressurized liquid extraction PLE , was validated by comparison with the concentration values from the NIST 1944 standard reference material. The advantages of the methods include low detection limits, PBDE congeners specificity using selected multiple reaction monitoring MRM transitions, and the absence of thermal degradation of higher PBDE congeners, especially BDE 209. The methods were applied for the determination of the above reported flame retardants in sewage sludge in order to get more information about the degradation on PBDEs in particular BDE 209 during municipal wastewater treatments. 1217 Mascolo G., Locaputo V., Mininni G. J. Chromatogr. A, 2010, 1217, 27, 4601 4611. 2010_J_Chrom_A_.pdf Articolo in rivista Elsevier 0021 9673 Journal of chromatography Print Journal of chromatography Print J. chromatogr. Print Journal of chromatography. Print Journal of chromatography. A Print giuseppe.mininni MININNI GIUSEPPE giuseppe.mascolo MASCOLO GIUSEPPE TA.P07.002.002 Sviluppo di nuovi processi di controllo dell inquinamento idrico. |
