Copyright 2012 Bruker Corporation. All Rights Reserved. Chemical and Applied Markets Ultra-sensitive Detection of Pharmaceutical and Personal Care Products (PPCPs) in Water with an Integrated On-Line Extraction-UHPLC-MS/MS System Helen Sun, Ph.D. Bruker Corporation, Chemical and Applied Markets (CAM)
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Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Ultra-sensitive Detection of Pharmaceutical and Personal Care Products (PPCPs) in Water with an
Integrated On-Line Extraction-UHPLC-MS/MS System
Helen Sun, Ph.D.
Bruker Corporation,
Chemical and Applied Markets (CAM)
Copyright 2012 Bruker Corporation. All Rights Reserved.
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Bruker LC-TQ Advantage
Advance HPLC, UHPLC (15,000 psi), & UHPLC-OLE (3 pumps in same cabinet) configuration
with built-in column oven and low dead-volume (60uL)
Industry work-horse PAL auto-sampler Vacuum insulated probe - Heated ESI
(VIP-HESI) with Active Exhaust for high-flow sensitivity & robustness
Dual inter-laced Ion funnels for sustained high-sensitivity
Lens-free collision cell design for maximum productivity
Detector technology for fast pos/neg switching & excellent negative ion
performance
Designed for a singular purpose – to reliably quantify thousands of real samples in the fastest ‘sample-to-report’ time possible
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
The Bruker LC-TQ Advantage Food Testing –Clenbuterol as a contaminant in meat
• Clenbuterol is a sympathomimetic amine (beta-2 agonist). • Side-effect is an increases in basal metabolism rates, which
helps build muscle mass, while reducing body-fat. • Major outbreak in China which sickened over 900 people • Over 17 livestock houses closed in Mexico due to 100% of
samples testing positive for clenbuterol
• EVOQ LC-TQ Advantage • Turn-key method on the EVOQ LC-TQ • Sustained high sensitivity –proof statement available • Available in Compound Based Screening library Day 1
Day 2
Day 3
Day 4
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Advance UHPLCOLE Pump configuration: Single Trap
Waste
CTC
MS
Column Oven
A B
Wash In
Wash Out
A B Solvent A
Solvent B
Mixer Purge valve
Purge out
OLE solvent
Purge valve
Waste
1
2
3 4
5
6
1
2
3
4
5 6
7
8
9
10
Maximum Pressure: 100 Mpa/1000 bar/15,000 psi
OLE loading mode
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Advance UHPLCOLE Pump configuration: Single Trap
Waste
CTC
MS
Column Oven
A B
Wash In
Wash Out
A B Solvent A
Solvent B
Mixer Purge valve
Purge out
OLE solvent
Purge valve
Waste
1
2
3 4
5
6
1 2
3
4
5 6
7
8
9
10
Maximum Pressure: 100 Mpa/1000 bar/15,000 psi
OLE analyzing mode
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Waste
CTC
MS
Column Oven
A B
Wash In
Wash Out
A B Solvent A
Solvent B
Mixer Purge valve
Purge out
OLE solvent
Purge valve
1
2
3 4
5
6
Waste
1
2
3
4
5 6
7
8
9
10
Advance UHPLCOLE Pump configuration: Dual Trap
Analyzing Trap 1 Loading Trap 2
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Waste
CTC
MS
Column Oven
A B
Wash In
Wash Out
A B Solvent A
Solvent B
Mixer Purge valve
Purge out
OLE solvent
Purge valve
1
2
3 4
5
6
Waste
1 2
3
4
5 6
7
8
9
10
Advance UHPLCOLE Pump configuration: Dual Trap
Loading Trap 1 Analyzing Trap 2
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EVOQ OLE – lowering detection limit
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EVOQ OLE application – PPCP quantitation in city tap water samples and river water
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
PPCP compounds Category Alprazolam anxiolytic
Ciproxacin antibiotic
Sulfamethoxazole antibiotic
Trimethoprim antibiotic
Carbamazepine anticonvulsant
2,4-D pesticide/herbicide
Ametryn pesticide/herbicide
Atrazine pesticide/herbicide
Bentazone pesticide/herbicide
Carboxine pesticide/herbicide
Cyanazine pesticide/herbicide
Diuron pesticide/herbicide
Hexazinone pesticide/herbicide
Hydroxy Atrazine pesticide/herbicide
MCPA pesticide/herbicide
Mecoprop pesticide/herbicide
Metolachlor pesticide/herbicide
Metribuzin pesticide/herbicide
Prometryn pesticide/herbicide
Pyriproxyfen pesticide/herbicide
Simazine pesticide/herbicide
Thiabendazole pesticide/parasiticide
Dapoxetine prescription drug
Sildenafil prescription drug
Caffeine stimulant
PPCP list
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Experimental condition
• LC
OLE pump • Flow rate: 500 µL/min • Gradient: isocratic, 100% H2O + 0.1% FA • Column: YMC-Pack Pro ODS-AQ,
• HESI: ±4000 V • Cone gas flow: 15 unit • Cone temp: 300 °C • Heated Probe gas: 50 unit • Heated Probe temp: 450 °C • Nebulizer gas flow: 50 unit • Exhaust gas: on
• Sample preparation • Water sample acidified to
0.1% FA and filtered (0.45µm)
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Selected PPCPs at 2 ppt
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Linearity, 1 ppt – 100 ppt
Trimethoprim
R2=0.999
Carbamazepine R2=0.999
Naproxen R2=0.999
Triclosan
R2=0.998
Gemfibrozil
R2=0.997
Sulfamethoxazole R2=0.999
Copyright 2012 Bruker Corporation. All Rights Reserved.
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Hexazinone
• Broad spectrum herbicide • Inhibits photosynthesis • Used to control grasses,
wood plants • High water solubility • A pervasive groundwater
contaminant
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Metolachlor
• Chloroacetanilide herbicide • Has been detected in ground
and surface water through out US (0.08 – 4.5 ppb)
• Category C pesticide by US EPA • Bioaccumulation of
metolachlor in edible species of fish
• US EPA health advisory level (HAL): 0.525 ppm
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Summary
• EVOQ OLE system provides a total solution for trace PPCP quantitation in water samples: automatic online extraction followed by LC-MS/MS targeted analysis
• An MRM based LC-MS/MS method has been developed for PPCP quantitation in city water, creek water and bottled water samples
• Quantitation result shows that the water quality between cities is slightly different, weed killer herbicides were screened in the tested water samples, but the concentration is still within safety range
• EVOQ OLE system is a ease-of-use, sensitive and robust instrument for PPCP analysis in water samples
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Conclusion
GC-TQ or LC-TQ MRM Data Reports
Data Generation Information Creation Decisions
Game-Changing Products for Quadrupole MS Applications