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![Page 1: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/1.jpg)
ZweckverbandLandeswasserversorgung
HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis
Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber
Zweckverband Landeswasserversorgung Laboratory for Operation Control and Research
Langenau, Germany
Club de CCM - 15èmeannée 6 Juin 2013
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ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
![Page 3: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/3.jpg)
ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
![Page 4: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/4.jpg)
ZweckverbandLandeswasserversorgung
Landeswasserversorgung is situated in South Germany
www.wikipedia.de
Paris Langenau
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ZweckverbandLandeswasserversorgung
Distribution area in South West Germany
3 Million customers within distribution area
Long-distance water fraction approx. 50%
Distribution area of LW Pipelines of LW N
Hessen Bayern
Rheinland-Pfalz
Frankreich
Schweiz Österreich
Heidel- berg
Tauber- bischofsheim
Bad Mergentheim
Crailsheim Schwäb. Hall Karlsruhe
Heilbronn
Pforzheim
Stuttgart Tübingen
Baden- Baden
Freuden- stadt
Aalen
Ulm Reutlingen
Offen- burg
Rottweil
Freiburg Tuttlingen
Biberach
Ravensburg
Friedrichshafen Singen
Lörrach
Konstanz
Bayern
SBH Osterbuch SBH Aufhausen
Egau- Wasserwerk
VPW Burgberg VPW Niederstotzingen WW Langenau
RWP Leipheim
SBH Amstetten
WW Blaubeuren
SBH Heuberg
BH Schönbühl
Distribution area of LW in South West Germany
Langenau Waterworks
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ZweckverbandLandeswasserversorgung
Danube water treatment
Ground water Blaubeuren Ground water Burgberg Spring water Egau waterworks
Groundwater Donauried
External sources
90
80
70
60
50
40
30
20
10
0
Million m3 / Year
2007 1999 2000 2001 2002 2003 2004 2005 2006
100 92,0
2008
4,7
28,0
18,7
9,9
2,7
28,0
4,0
31,2
18,5
10,0
3,0
26,2
92,9
4,0
28,0
16,1
10,9
3,1
31,3 93,4 94,0
29,2
3,0
10,8
16,7
30,3
4,0 4,2 4,1 3,7
32,5
17,4
11,3 4,0
32,9 102,3
27,0
15,0
11,0
3,2
38,3 98,6
27,9
15,6
9,2
2,6
37,0 96,0
3,7
29,8
15,4
7,4
2,7
36,1 95,1
3,4
28,5
15,5
6,6
2,5
37,3 93,8
3,4
32,0
17,4 3,4
2,1
33,4 91,7
Water treatment from different resources
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ZweckverbandLandeswasserversorgung
Contact Slurry
Slurry Treatment
Slurry Treatment
Groundwater decarbonized
Groundwater
Amstetten
Osterbuch
Activated Carbon
Flocculation - agent (Fe +++ ) Lime Milk Flocculation aid
Flocculation - agent (Fe +++ )
Lime Milk
Flocculation aid
Ozone
Flocculation - agent (Fe +++ )
Hydroanthrazit Quarz sand Donau
Chlorine dioxide
Chlorine dioxide Orthophosphate
Raw Water Pump Station
Filtrate Tank Pure Water Tank Pump Station
Filter Unit Ozonation Unit
Flocculation Unit 1 Raw Water Tank
Pre-mixing Unit Flocculation Unit 2
Q FL2 Q FL1
Danube
Treatment of Danube water at Langenau waterworks
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ZweckverbandLandeswasserversorgung
Drin
king
Wat
er, G
roun
dwat
er
Sur
face
Wat
er
Detection Separation Enrichment
Solid Phase Extraction
Light phase perforator
UV-Scan
Toxicity
MS MS/MS
ECD, FID, PND
Liquid/Liquid-Extraction
SEC
HPTLC
CC
HPTLC
GC
HPLC
Clean-up
„Multidimensional Screening“
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ZweckverbandLandeswasserversorgung
Drin
king
Wat
er, G
roun
dwat
er
Sur
face
Wat
er
Detection Separation Enrichment
Solid Phase Extraction
Light phase perforator
UV-Scan
Toxicity
MS MS/MS
ECD, FID, PND
Liquid/Liquid-Extraction
SEC
HPTLC
CC
HPTLC
GC
HPLC
Clean-up
„Multidimensional Screening“
![Page 10: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/10.jpg)
ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
![Page 11: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/11.jpg)
ZweckverbandLandeswasserversorgung
Map of ground water monitoring wells in the water protection area
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ZweckverbandLandeswasserversorgung
60 µl TBME-Extrakt
0
100
200
300
400
500
600
700
800
0 0.125 0.25 0.375 0.5 0.625 0.75 0.875 1Rf
AU
190 nm200 nm220 nm240 nm260 nm280 nm300 nm
Schematic diagram of the HPTLC/AMD analysis
Development AMD 2
Detection Scanner 3
Application TLC Sampler 4
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ZweckverbandLandeswasserversorgung
HPTLC/AMD fingerprint of a ground water sample
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ZweckverbandLandeswasserversorgung
? HPTLC/AMD fingerprint of a ground water sample
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ZweckverbandLandeswasserversorgung
nano-Electrosprayion source
Quadrupole
Flight tubewith reflector
Tandem mass spectrometerwith full-scan capabilityMass accuracy: 2 ppm
Eluent from HPLC pump
H. Luftmann (2004) Anal. Bioanal Chem., 378, 964
Transfer of substances via HPTLC-MS interface and MS analysis
Plunger with cutting edge and filter frit
Seal with carrier material
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ZweckverbandLandeswasserversorgung
m/z 173.0379 Molecular formular:C8H10N2O4S
Asulam (Herbicide)
Identification via HPLC-qTOF/MS
Confirmed by reference
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ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
![Page 18: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/18.jpg)
ZweckverbandLandeswasserversorgung
Direct abstraction of Danube water in the downstream of the Cities of Ulm and Neu-Ulm
Neu-Ulm
Ulm
Langenau
Günzburg
Leipheim
Wiblingen
Erbach
Dellmensingen
Abstraction point
To waterworks Langenau
Central sewage treatment plant
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ZweckverbandLandeswasserversorgung
Time variation curve of Benzotriazoles in the Danube (Leipheim, 2010)
N = 359
Con
cent
ratio
n in
ng/
L
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ZweckverbandLandeswasserversorgung
Contact Slurry
Slurry Treatment
Slurry Treatment
Groundwater decarbonized
Groundwater
Amstetten
Osterbuch
Activated Carbon
Flocculation - agent (Fe +++ ) Lime Milk Flocculation aid
Flocculation - agent (Fe +++ )
Lime Milk
Flocculation aid
Ozone
Flocculation - agent (Fe +++ )
Hydroanthrazit Quarz sand Donau
Chlorine dioxide
Chlorine dioxide Orthophosphate
Raw Water Pump Station
Filtrate Tank Pure Water Tank Pump Station
Filter Unit Ozonation Unit
Flocculation Unit 1 Raw Water Tank
Pre-mixing Unit Flocculation Unit 2
Q FL2 Q FL1
Danube
Treatment of Danube water at Langenau waterworks
![Page 21: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/21.jpg)
ZweckverbandLandeswasserversorgung
Contact Slurry
Slurry Treatment
Slurry Treatment
Groundwater decarbonized
Groundwater
Amstetten
Osterbuch
Activated Carbon
Flocculation - agent (Fe +++ ) Lime Milk Flocculation aid
Flocculation - agent (Fe +++ )
Lime Milk
Flocculation aid
Ozone
Flocculation - agent (Fe +++ )
Hydroanthrazit Quarz sand Donau
Chlorine dioxide
Chlorine dioxide Orthophosphate
Raw Water Pump Station
Filtrate Tank Pure Water Tank Pump Station
Filter Unit Ozonation Unit
Flocculation Unit 1 Raw Water Tank
Pre-mixing Unit Flocculation Unit 2
Q FL2 Q FL1
Danube
Treatment of Danube water at Langenau waterworks
![Page 22: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/22.jpg)
ZweckverbandLandeswasserversorgung
Schematic illustration of the experimental ozonation reactor
NH
NN
CH3
+ O3 ?
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ZweckverbandLandeswasserversorgung
Separation of the main ozonation products via „2D-chromatograpy“
Sample
HPLC (RP)
HPTLC/AMD (NP)
HPTLC/AMD (NP)
Derivatization
HPLC-QTOF/MS
HPLC-QTOF/MS
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ZweckverbandLandeswasserversorgung
Separation of HPLC-fractions via HPTLC/AMD (λ = 254 nm)
λ = 254 nm La
ufst
reck
e
HPLC Fractions
1 2 3 4 5 6
Mig
ratio
n
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ZweckverbandLandeswasserversorgung
[M+H]+268.3
[M+Na]+290.3
0.0
0.2
0.4
0.6
0.8
1.0
Intens.
1.0
x108
150 200 250 300 350 400 m/z
[M+H]+268.3
[M+Na]+290.3
0.0
0.2
0.4
0.6
0.8
1.0
Intens.
1.0
x108
150 200 250 300 350 400 m/z
H. Luftmann (2004), Anal. Bioanal Chem., 378, 964
Schematic diagram of the HPTLC-MS coupling Development
AMD 2 Transfer and Detection
TLC-MS interface and ESI-MS Application
TLC Sampler 4
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ZweckverbandLandeswasserversorgung
Localisation of the postulated oxidation product M147 on the developed HPTLC plate
Proposed structure
Retention time
Inte
nsity
[cou
nts]
Inte
nsity
[cou
nts]
Mass spectrum
Mig
ratio
n
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ZweckverbandLandeswasserversorgung
Confirmation of the carbonyl group with 2,4-DNPH*
NN
NH
N
NH
NO2O2N
NN
NH
OH
NH2
NH
NO2O2N
+H2SO4
-H2O
M = 147,0433 Da [M-H]- = 146,0360 Da
M = 327,0716 Da [M-H]- = 326,0643 Da
M = 198,0389 Da [M-H]- = 197,0316 Da
* 2,4-Dinitrophenylhydrazin
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ZweckverbandLandeswasserversorgung
Confirmation of the carbonyl group with 2,4-DNPH
Extraction of the derivatization product (m/z 326) for the oxidation product M147
Retention time
Inte
nsity
[cou
nts]
Inte
nsity
[cou
nts]
Mig
ratio
n
Mass spectrum
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ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
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ZweckverbandLandeswasserversorgung
Luminescence bacteria Vibrio Fischeri
• Marine bacterium
• Lives in symbiosis with marine life forms
• Continuous bioluminescence
• Bioluminescence is coupled to
energy metabolism
Inhibition of electron transport Isolation
Narcotic effects
Suspension of Vibrio fischeri in water
Reference: Reinecke, N. (2003), Dissertation, Universität Hamburg
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ZweckverbandLandeswasserversorgung
Contact Slurry
Slurry Treatment
Slurry Treatment
Groundwater decarbonized
Groundwater
Amstetten
Osterbuch
Activated Carbon
Flocculation - agent (Fe +++ ) Lime Milk Flocculation aid
Flocculation - agent (Fe +++ )
Lime Milk
Flocculation aid
Ozone
Flocculation - agent (Fe +++ )
Hydroanthrazit Quarz sand Donau
Chlorine dioxide
Chlorine dioxide Orthophosphate
Raw Water Pump Station
Filtrate Tank Pure Water Tank Pump Station
Filter Unit Ozonation Unit
Flocculation Unit 1 Raw Water Tank
Pre-mixing Unit Flocculation Unit 2
Q FL2 Q FL1
Danube
Treatment of Danube water at Langenau waterworks
![Page 32: HPTLC/AMD-EDA - HPLC-qTOF/MS in water and ... Landeswasserversorgung HPTLC/AMD-EDA - HPLC-qTOF/MS in water and environment analysis Stefan C. Weiss, Wolfgang Schulz and Walter H. Weber](https://reader031.fdocuments.us/reader031/viewer/2022013014/5b04e0497f8b9a89208e4be9/html5/thumbnails/32.jpg)
ZweckverbandLandeswasserversorgung
10 min
pH3 pH8 pH3 pH8
Metoprolol Propranolol
200µl 200µl 100µl 100µl
Standards
M P 134 ng/µl 10 ng/µl
O
OH
NH
CH3
CH3
OCH3
Ozonation by-products of ß-blockers
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ZweckverbandLandeswasserversorgung
10 min
CH3N
N
O
Cl
NH2
Ozonation by-products of the main metabolite of the pesticide Chloridazon
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ZweckverbandLandeswasserversorgung
Potential ground water contamination by synthetic turfs
500 µl500 µl
Leaching test: (analog DIN 38414-S4)
Elution of 40 g sample with 80 g water Duration: 24 h Liquid/liquid extraction of the eluate Extraction solvent: MTBE Blank: Ultra pure water
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ZweckverbandLandeswasserversorgung
Fingerprint of waste water samples (Δt = 6 month)
2. Sample series 1. Sample series
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ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
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ZweckverbandLandeswasserversorgung
Ref.: Google Maps
Ground water Catchment
Aerial photo of the region of interest
Sports field
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ZweckverbandLandeswasserversorgung
Simulation of leaching synthetic turf with water
Leaching test: (analog DIN 38414-S4)
Elution of 40 g sample with 80 g water Duration: 24 h Liquid/liquid extraction of the eluate Extraction solvent: Tert-butyl-methyl-ether Blank: Ultra pure water
Synthetic turf:
PUR rubber granulate (elastic layer)
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Weisemann, C., Kreiss, W., Rast, H-G., Eberz. G.;“Analytical Method for Investigating Mixtures for Toxic Components.” European Patent No: EP 0 588 139 B1.
Development AMD 2
Immersion Vibrio fischeri
Application TLC Sampler 4
Detection Bioluminizer
Schematic diagram for the HPTLC-AMD analysis with bioluminescence detection
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ZweckverbandLandeswasserversorgung
HPTLC/AMD analysis
Eluents: MeOH:NH3 (4%) Dichloromethane n-Hexane
Chromatography:
Detection: - UV absorption (multiple wavelength scan) - Fluorescence quenching at 254 nm - Fluorescence, excitation at 366 nm - Luminescence inhibition test
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Detection of luminescence inhibition (Vibrio fischeri)
Rf =1
Rf =0
λ = 254 nm
Bla
nk e
xtra
ct
20 µ
l TB
ME
extr
act
40 µ
l TB
ME
extr
act
60 µ
l TB
ME
extr
act
Bla
nk tr
ack
Ref
eren
ce M
ix
Publication in Preparation
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ZweckverbandLandeswasserversorgung
InhibitionInhibition−
=Γ100
Gamma-Value:
Gamma value chromatogram (proportional to luminescence inhibition)
40 µl TBME extract
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ZweckverbandLandeswasserversorgung
[M+H]+268.3
[M+Na]+290.3
0.0
0.2
0.4
0.6
0.8
1.0
Intens.
1.0
x108
150 200 250 300 350 400 m/z
[M+H]+268.3
[M+Na]+290.3
0.0
0.2
0.4
0.6
0.8
1.0
Intens.
1.0
x108
150 200 250 300 350 400 m/z
H. Luftmann (2004), Anal. Bioanal Chem., 378, 964
Schematic diagram of the HPTLC-MS coupling Development
AMD 2 Transfer and Detection
TLC-MS interface and ESI-MS Application
TLC Sampler 4
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ZweckverbandLandeswasserversorgung
0
200
400
600
800
1000
4 5 6 7 8 9 10 11 12 13
Retentionszeit [min]
Mas
se
Non-Target-Screening via LC-QTOF
EIC: 143.0502
Retentionszeit [min] 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Inte
nsitä
t
TIC
EIC: 695.3117
EIC: 430.9735
EIC: 242.0129
0
800
700
600
500
400
300
200
100
m/z
EIC: 143.0502
Retentionszeit [min] 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Inte
nsitä
t
TIC
EIC: 695.3117
EIC: 430.9735
EIC: 242.0129
0
800
700
600
500
400
300
200
100
m/z
522 Compounds
Nano-LC
QTOF
Top view
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ZweckverbandLandeswasserversorgung
Mass/Retention time diagram of all compounds in the eluate
522 Komponenten
Einzeichnen von Benzothiazolen
Publication in Preparation
Mas
s
Retention time [min]
522 Compounds
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ZweckverbandLandeswasserversorgung
Rf =1
Rf =0
NP
RP
HP
TLC
HPLC
Bioluminescence detection
Detection of luminescence inhibition (Vibrio fischeri) and transfer of the substances via HPTLC-MS interface to MS
Publication in Preparation
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ZweckverbandLandeswasserversorgung
0
10
20
30
40
50
60
70
80
90
100
200 250 300 350 400 450 500 550 600
Abs
orpt
ion
0
10
20
30
40
50
60
70
80
90
100
200 250 300 350 400 450 500 550 600
Abso
rptio
n
Identification of the unknown compound
UV/VIS
λ [nm]
λ [nm]
137.0243 (M+H) + 137.0243
(M+H) +
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
137.0243 (M+H) + 138.0276
(M+H) +
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
137.0243 (M+H) + 137.0243
(M+H) +
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
3 x10
0
1
2
3
4
5
6
7
8 136.0213 (M+H) +
Counts vs. Mass - to - Charge ( m/z ) 136 136.5 137 137.5 138
137.0243 (M+H) + 138.0276
(M+H) +
Empirical formula: C7H5NS
137.0245 ( M+H) + 138.0276
( M+H) +
5 x10
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1 136.0216 ( M+H) +
Counts vs. Mass - to - Charge (m/z) 136 136.5 137 137.5 138
5 x10
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1 136.0216 ( M+H) +
Counts vs. Mass - to - Charge (m/z) 136 136.5 137 137.5 138
137.0245 ( M+H) + 138.0276
( M+H) +
MS
Reference
Sample
Database query Database query
Benzothiazole
N
S
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Rf =1
Rf =0
NP
RP
HP
TLC
HPLC
Bioluminescence detection
Detection of luminescence inhibition (Vibrio fischeri) and transfer of the substances via HPTLC-MS interface to MS
Publication in Preparation
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ZweckverbandLandeswasserversorgung
0
10
20
30
40
50
60
70
80
90
100
200 250 300 350 400 450 500 550 600[ ]
Abs
orpt
ion
UV/VIS
λ [nm]
λ [nm]
Empirical formula: C7H5NOS MS
Reference
Sample
Database query Database query
N
SOH
2-Hydroxybenzothiazole
Identification of the unknown compound (II)
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Mass/Retention time diagram of all compounds in the eluate
522 Komponenten
Einzeichnen von Benzothiazolen
N
S
N
SNH2
N
SOH
Benzothiazole
2-Aminobenzothiazole
2-Hydroxybenzothiazole
l
Publication in Preparation
Mas
s
Retention time [min]
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ZweckverbandLandeswasserversorgung
Target Analysis for Benzothiazole via Triple Quadrupol MS
1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0Time, min
0.0
5.0e5
1.0e6
1.5e6
2.0e6
2.5e6
3.0e6
3.5e6
4.0e6
4.5e6
5.0e65.2e6
2-Aminobenzothiazole
2-Hydroxybenzothiazole
2-(Methylthio)-benzothiazole
2-Mercaptobenzothiazole
Eluate of the elastic layer Q1 q2 Q3
N
SOH
N
SNH2
N
SSH
N
SS CH3
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ZweckverbandLandeswasserversorgung
Rf =1
Rf =0
NP
RP
HP
TLC
HPLC
Detection of luminescence inhibition (Vibrio fischeri) and transfer of the substances via HPTLC-MS interface to MS
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Combination of the Non-Target-Screening Strategies
Rf =1
Rf =0
Sportplatzbelag HPTLC-Extrakt bei 36 mm
0
200
400
600
800
1000
4 5 6 7 8 9 10 11 12 13
Retentionszeit [min]
Mas
se
52 Compounds
Publication in Preparation
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ZweckverbandLandeswasserversorgung
Mass spectra from the HPTLC zone with a migration distance of 36 mm
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ZweckverbandLandeswasserversorgung
Mass/Retention time diagram of all compounds in the eluate
522 Komponenten
Einzeichnen von Benzothiazolen
N
S
N
SNH2
N
SOH
Benzothiazol
2-Aminobenzothiazol
2-Hydroxybenzothiazol
Unknown Substance
Mas
s
Retention time [min]
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ZweckverbandLandeswasserversorgung
MS/MS from the HPTLC zone with a migration distance of 36 mm 4 x10
0 0,2 0,4 0,6 0,8
1 1,2 1,4 1,6 1,8
2 2,2 2,4 2,6 2,8
3 3,2 3,4 3,6 3,8
4 4,2 4,4 4,6 4,8
…
123.0663 193.1192
Counts vs. Mass-to-Charge (m/z) 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460
177.0880
5 x10
0 0.25 0.5
0.75 1
1.25 1.5
1.75 2
2.25 2.5
2.75 3
3.25 3.5
3.75 4
4.25 4.5
4.75 5
5.25 5.5
5.75 6
6.25 6.5
6.75 7
7.25 7.5
7.75 8
8.25 8.5
8.75 9
9.25 9.5 359.2047
360.2070
Counts vs. Mass-to-Charge (m/z) 358.4 358.6 358.8 359 359.2 359.4 359.6 359.8 360 360.2 360.4 360.6 360.8 361 361.2 361.4 361.6 361.8 362
MS/MS
MS
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ZweckverbandLandeswasserversorgung
1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0Time, min
0.0
000.0
1.0e4
1.5e4
2.0e4
2.5e4
3.0e4
3.5e4
4.0e4
4.5e4
5.0e4
5.5e4
6.0e4
6.5e4
7.0e4
7.5e4
Water from the ground water catchment Q1 q2 Q3
Target Analysis for Benzothiazole via Triple Quadrupol MS
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ZweckverbandLandeswasserversorgung
1 2 3 4 5 6 7 8 9 10 11 12 13 14Time, min
0.0
5.0e5
1.0e6
1.5e6
2.0e6
2.5e6
3.0e6
3.5e6
4.0e6
4.5e6
5.0e6
5.5e6
6.0e6
6.5e6
7.0e6
7.5e6
8.0e6
8.5e6
Mass transition 359.2 / 177
359.2 177
Eluate of the elastic layer
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ZweckverbandLandeswasserversorgung
1 2 3 4 5 6 7 8 9 10 11 12 13 14Time, min
0.0
5.0e5
1.0e6
1.5e6
2.0e6
2.5e6
3.0e6
3.5e6
4.0e6
4.5e6
5.0e6
5.5e6
6.0e6
6.5e6
7.0e6
7.5e6
8.0e6
8.5e6
Eluat
1 2 3 4 5 6 7 8 9 10 11 12 13 14Time, min
0
20
40
60
80
100
120
140
160
180
200
220
240
260
280
300
320
340
360
380
400
420
440
460
0.170.53
359.2 177
Dilution factor > 50000
Mass transition 359.2 / 177
Water from the ground water catchment
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ZweckverbandLandeswasserversorgung
Content
Introduction
Ground water contamination from synthetic turf
Identification of pesticides in ground water
Effect-Directed Analysis with Vibrio fischeri
Ozonation reaction products
Conclusion
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ZweckverbandLandeswasserversorgung
Conclusion
1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0Time, min
0.0
000.0
1.0e4
1.5e4
2.0e4
2.5e4
3.0e4
3.5e4
4.0e4
4.5e4
5.0e4
5.5e4
6.0e4
6.5e4
7.0e4
7.5e4
1 2 3 4 5 6 7 8 9 10 11 12 13 14Time, min
0
20
40
60
80
100
120
140
160
180
200
220
240
260
280
300
320
340
360
380
400
420
440
460
0.170.53
359.2 / 177
Rf = 0
Rf = 1
3.0 2.5 2.0 1.5 1.0 0.5
Γ-Wert
N
S
Unknown Substance
Benzothiazole
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ZweckverbandLandeswasserversorgung
Alexander Müller and the member of staff at the Laboratory for Operation Control and Research
Acknowledgments
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ZweckverbandLandeswasserversorgung
Thank you for your attention!