Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples
Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analys...
Ausführliche Beschreibung
Gespeichert in:
| Autor*in: |
Ciofi, Lorenzo [verfasserIn] |
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| Format: |
E-Artikel |
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| Sprache: |
Englisch |
| Erschienen: |
2016 |
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| Schlagwörter: |
On-line solid phase extraction–liquid chromatography–tandem mass spectrometry |
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| Anmerkung: |
© Springer-Verlag Berlin Heidelberg 2016 |
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| Übergeordnetes Werk: |
Enthalten in: Analytical and bioanalytical chemistry - Berlin : Springer, 2002, 408(2016), 12 vom: 20. Feb., Seite 3331-3347 |
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| Übergeordnetes Werk: |
volume:408 ; year:2016 ; number:12 ; day:20 ; month:02 ; pages:3331-3347 |
| Links: |
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| DOI / URN: |
10.1007/s00216-016-9403-5 |
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| Katalog-ID: |
SPR002244152 |
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| 100 | 1 | |a Ciofi, Lorenzo |e verfasserin |4 aut | |
| 245 | 1 | 0 | |a Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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| 520 | |a Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites | ||
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| 650 | 4 | |a Alkylphenols polyethoxylates |7 (dpeaa)DE-He213 | |
| 650 | 4 | |a Alkylphenoxy carboxylates |7 (dpeaa)DE-He213 | |
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| 700 | 1 | |a Ancillotti, Claudia |4 aut | |
| 700 | 1 | |a Chiuminatto, Ugo |4 aut | |
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| 700 | 1 | |a Pasquini, Benedetta |4 aut | |
| 700 | 1 | |a Bruzzoniti, Maria Concetta |4 aut | |
| 700 | 1 | |a Rivoira, Luca |4 aut | |
| 700 | 1 | |a Del Bubba, Massimo |4 aut | |
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10.1007/s00216-016-9403-5 doi (DE-627)SPR002244152 (SPR)s00216-016-9403-5-e DE-627 ger DE-627 rakwb eng Ciofi, Lorenzo verfasserin aut Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples 2016 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © Springer-Verlag Berlin Heidelberg 2016 Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 Ancillotti, Claudia aut Chiuminatto, Ugo aut Fibbi, Donatella aut Pasquini, Benedetta aut Bruzzoniti, Maria Concetta aut Rivoira, Luca aut Del Bubba, Massimo aut Enthalten in Analytical and bioanalytical chemistry Berlin : Springer, 2002 408(2016), 12 vom: 20. Feb., Seite 3331-3347 (DE-627)25372337X (DE-600)1459122-4 1618-2650 nnns volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 https://dx.doi.org/10.1007/s00216-016-9403-5 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER SSG-OLC-PHA GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_206 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2070 GBV_ILN_2086 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2116 GBV_ILN_2118 GBV_ILN_2119 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2360 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4012 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4277 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 408 2016 12 20 02 3331-3347 |
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10.1007/s00216-016-9403-5 doi (DE-627)SPR002244152 (SPR)s00216-016-9403-5-e DE-627 ger DE-627 rakwb eng Ciofi, Lorenzo verfasserin aut Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples 2016 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © Springer-Verlag Berlin Heidelberg 2016 Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 Ancillotti, Claudia aut Chiuminatto, Ugo aut Fibbi, Donatella aut Pasquini, Benedetta aut Bruzzoniti, Maria Concetta aut Rivoira, Luca aut Del Bubba, Massimo aut Enthalten in Analytical and bioanalytical chemistry Berlin : Springer, 2002 408(2016), 12 vom: 20. Feb., Seite 3331-3347 (DE-627)25372337X (DE-600)1459122-4 1618-2650 nnns volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 https://dx.doi.org/10.1007/s00216-016-9403-5 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER SSG-OLC-PHA GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_206 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2070 GBV_ILN_2086 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2116 GBV_ILN_2118 GBV_ILN_2119 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2360 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4012 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4277 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 408 2016 12 20 02 3331-3347 |
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10.1007/s00216-016-9403-5 doi (DE-627)SPR002244152 (SPR)s00216-016-9403-5-e DE-627 ger DE-627 rakwb eng Ciofi, Lorenzo verfasserin aut Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples 2016 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © Springer-Verlag Berlin Heidelberg 2016 Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 Ancillotti, Claudia aut Chiuminatto, Ugo aut Fibbi, Donatella aut Pasquini, Benedetta aut Bruzzoniti, Maria Concetta aut Rivoira, Luca aut Del Bubba, Massimo aut Enthalten in Analytical and bioanalytical chemistry Berlin : Springer, 2002 408(2016), 12 vom: 20. Feb., Seite 3331-3347 (DE-627)25372337X (DE-600)1459122-4 1618-2650 nnns volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 https://dx.doi.org/10.1007/s00216-016-9403-5 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER SSG-OLC-PHA GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_206 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2070 GBV_ILN_2086 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2116 GBV_ILN_2118 GBV_ILN_2119 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2360 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4012 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4277 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 408 2016 12 20 02 3331-3347 |
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10.1007/s00216-016-9403-5 doi (DE-627)SPR002244152 (SPR)s00216-016-9403-5-e DE-627 ger DE-627 rakwb eng Ciofi, Lorenzo verfasserin aut Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples 2016 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © Springer-Verlag Berlin Heidelberg 2016 Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 Ancillotti, Claudia aut Chiuminatto, Ugo aut Fibbi, Donatella aut Pasquini, Benedetta aut Bruzzoniti, Maria Concetta aut Rivoira, Luca aut Del Bubba, Massimo aut Enthalten in Analytical and bioanalytical chemistry Berlin : Springer, 2002 408(2016), 12 vom: 20. Feb., Seite 3331-3347 (DE-627)25372337X (DE-600)1459122-4 1618-2650 nnns volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 https://dx.doi.org/10.1007/s00216-016-9403-5 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER SSG-OLC-PHA GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_206 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2070 GBV_ILN_2086 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2116 GBV_ILN_2118 GBV_ILN_2119 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2360 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4012 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4277 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 408 2016 12 20 02 3331-3347 |
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10.1007/s00216-016-9403-5 doi (DE-627)SPR002244152 (SPR)s00216-016-9403-5-e DE-627 ger DE-627 rakwb eng Ciofi, Lorenzo verfasserin aut Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples 2016 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © Springer-Verlag Berlin Heidelberg 2016 Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 Ancillotti, Claudia aut Chiuminatto, Ugo aut Fibbi, Donatella aut Pasquini, Benedetta aut Bruzzoniti, Maria Concetta aut Rivoira, Luca aut Del Bubba, Massimo aut Enthalten in Analytical and bioanalytical chemistry Berlin : Springer, 2002 408(2016), 12 vom: 20. Feb., Seite 3331-3347 (DE-627)25372337X (DE-600)1459122-4 1618-2650 nnns volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 https://dx.doi.org/10.1007/s00216-016-9403-5 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER SSG-OLC-PHA GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_206 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2070 GBV_ILN_2086 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2116 GBV_ILN_2118 GBV_ILN_2119 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2360 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4012 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4277 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 408 2016 12 20 02 3331-3347 |
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Enthalten in Analytical and bioanalytical chemistry 408(2016), 12 vom: 20. Feb., Seite 3331-3347 volume:408 year:2016 number:12 day:20 month:02 pages:3331-3347 |
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On-line solid phase extraction–liquid chromatography–tandem mass spectrometry Alkylphenols polyethoxylates Alkylphenoxy carboxylates Alkylphenols Wastewater |
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Ciofi, Lorenzo @@aut@@ Ancillotti, Claudia @@aut@@ Chiuminatto, Ugo @@aut@@ Fibbi, Donatella @@aut@@ Pasquini, Benedetta @@aut@@ Bruzzoniti, Maria Concetta @@aut@@ Rivoira, Luca @@aut@@ Del Bubba, Massimo @@aut@@ |
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<?xml version="1.0" encoding="UTF-8"?><collection xmlns="http://www.loc.gov/MARC21/slim"><record><leader>01000caa a22002652 4500</leader><controlfield tag="001">SPR002244152</controlfield><controlfield tag="003">DE-627</controlfield><controlfield tag="005">20230519234715.0</controlfield><controlfield tag="007">cr uuu---uuuuu</controlfield><controlfield tag="008">201001s2016 xx |||||o 00| ||eng c</controlfield><datafield tag="024" ind1="7" ind2=" "><subfield code="a">10.1007/s00216-016-9403-5</subfield><subfield code="2">doi</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(DE-627)SPR002244152</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(SPR)s00216-016-9403-5-e</subfield></datafield><datafield tag="040" ind1=" " ind2=" "><subfield code="a">DE-627</subfield><subfield code="b">ger</subfield><subfield code="c">DE-627</subfield><subfield code="e">rakwb</subfield></datafield><datafield tag="041" ind1=" " ind2=" "><subfield code="a">eng</subfield></datafield><datafield tag="100" ind1="1" ind2=" "><subfield code="a">Ciofi, Lorenzo</subfield><subfield code="e">verfasserin</subfield><subfield code="4">aut</subfield></datafield><datafield tag="245" ind1="1" ind2="0"><subfield code="a">Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples</subfield></datafield><datafield tag="264" ind1=" " ind2="1"><subfield code="c">2016</subfield></datafield><datafield tag="336" ind1=" " ind2=" "><subfield code="a">Text</subfield><subfield code="b">txt</subfield><subfield code="2">rdacontent</subfield></datafield><datafield tag="337" ind1=" " ind2=" "><subfield code="a">Computermedien</subfield><subfield code="b">c</subfield><subfield code="2">rdamedia</subfield></datafield><datafield tag="338" ind1=" " ind2=" "><subfield code="a">Online-Ressource</subfield><subfield code="b">cr</subfield><subfield code="2">rdacarrier</subfield></datafield><datafield tag="500" ind1=" " ind2=" "><subfield code="a">© Springer-Verlag Berlin Heidelberg 2016</subfield></datafield><datafield tag="520" ind1=" " ind2=" "><subfield code="a">Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. 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Ciofi, Lorenzo |
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Ciofi, Lorenzo misc On-line solid phase extraction–liquid chromatography–tandem mass spectrometry misc Alkylphenols polyethoxylates misc Alkylphenoxy carboxylates misc Alkylphenols misc Wastewater Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples On-line solid phase extraction–liquid chromatography–tandem mass spectrometry (dpeaa)DE-He213 Alkylphenols polyethoxylates (dpeaa)DE-He213 Alkylphenoxy carboxylates (dpeaa)DE-He213 Alkylphenols (dpeaa)DE-He213 Wastewater (dpeaa)DE-He213 |
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misc On-line solid phase extraction–liquid chromatography–tandem mass spectrometry misc Alkylphenols polyethoxylates misc Alkylphenoxy carboxylates misc Alkylphenols misc Wastewater |
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misc On-line solid phase extraction–liquid chromatography–tandem mass spectrometry misc Alkylphenols polyethoxylates misc Alkylphenoxy carboxylates misc Alkylphenols misc Wastewater |
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misc On-line solid phase extraction–liquid chromatography–tandem mass spectrometry misc Alkylphenols polyethoxylates misc Alkylphenoxy carboxylates misc Alkylphenols misc Wastewater |
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Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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Ciofi, Lorenzo |
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Analytical and bioanalytical chemistry |
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Ciofi, Lorenzo Ancillotti, Claudia Chiuminatto, Ugo Fibbi, Donatella Pasquini, Benedetta Bruzzoniti, Maria Concetta Rivoira, Luca Del Bubba, Massimo |
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Elektronische Aufsätze |
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Ciofi, Lorenzo |
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10.1007/s00216-016-9403-5 |
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fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
| abstract |
Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites © Springer-Verlag Berlin Heidelberg 2016 |
| abstractGer |
Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites © Springer-Verlag Berlin Heidelberg 2016 |
| abstract_unstemmed |
Abstract Three different sorbents (i.e. endcapped octadecylsilane, octasilane and styrene-N-vinylpiperidinone co-polymer) were investigated in order to develop an on-line solid phase extraction–liquid chromatographic tandem mass spectrometric method (on-line SPE–LC–MS/MS) for the simultaneous analysis of alkylphenols polyethoxylate ($ AP_{n} $EOs, n = 1–8) and corresponding monocarboxylate ($ AP_{1} $ECs) and phenolic (APs) metabolites. The endcapped octadecylsilane was selected due to its full compatibility with a chromatographic approach, which allowed the elution of positively and negatively ionisable compounds in two distinct retention time windows, using a water–acetonitrile–tetrahydrofuran ternary gradient and a pellicular pentafluorophenyl column. On this SPE sorbent, the composition of the loading/clean-up solution was then optimized in order to achieve the best recoveries of target analytes. Under the best experimental conditions, the total analysis time per sample was 25 min and method detection limits (MDLs) were in the sub-nanograms per litre to nanograms per litre range (0.0081–1.0 ng $ L^{−1} $) for $ AP_{n} $EOs with n = 2–8, $ AP_{1} $ECs and APs, whereas for $ AP_{1} $EOs, an MDL of about 50 ng $ L^{−1} $ was found. Using the mass-labelled compound spiking technique, the method performance was tested on inlet and outlet wastewater samples from three activated sludge treatment plants managing domestic and industrial sewages of the urban areas and the textile district of Prato and Bisenzio valley (Tuscany, Italy); in most cases, apparent recovery percentages approximately in the ranges of 50–110 % and 80–120 % were found for inlet and outlet samples, respectively. The on-line SPE–LC–MS/MS analysis of wastewater samples highlighted the presence of target analytes at concentrations ranging from few nanograms per litre to thousands nanograms per litre, depending on the compound and matrix analysed. $ AP_{2} $ECs were also tentatively identified in outlet samples. Graphical AbstractGraphical representation of the on-line SPE-LC-MS/MS approach for the fully automated analysis of ethoxylated alkylphenols and their carboxylic and phenolic metabolites © Springer-Verlag Berlin Heidelberg 2016 |
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Fully automated on-line solid phase extraction coupled to liquid chromatography–tandem mass spectrometry for the simultaneous analysis of alkylphenol polyethoxylates and their carboxylic and phenolic metabolites in wastewater samples |
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| score |
7.4019194 |