Comparison of Modern LC- MS/MS Techniques for Analysis of TOrCs in Water. Tarun Anumol, Shane Snyder NEMC 2014
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1 Comparison of Modern LC- MS/MS Techniques for Analysis of TOrCs in Water Tarun Anumol, Shane Snyder NEMC 2014
2 Introduction
3 Science Advisory Board Current Trends
4 Current Trends
5 Automation
6 Traditional Extraction Techniques Analysis of TOrCs in Water
7 Analysis of TOrCs by C-SPE Sample collection and Transport Evaporation Surrogate addition Analysis Extraction (SPE) by Autotrace
8 Sample Transport
9 Sample Volume
10 Analysis of TOrCs by OSPE Surrogate Addition into 5 ml of sample Analysis (1700 µl injection volume)
11 Instrument Setup
12 Instrument Setup Agilent Flexcube connected to 6460 MS/MS
13 Large Volume Direct Injection Surrogate Addition into 1 ml of sample Analysis (100 µl injection volume)
14 Trace Organic Chemicals Atenolol (ß-blocker) Atrazine (Herbicide) Benzophenone (UV-blocker) Bisphenol A (plasticizer) Caffeine (stimulant) Carbamazepine (Anti-seizure) DEET (Insect-repellant) Dexamethasone (glucocorticoid) Trimethoprim (Antibiotic) Estrone (Hormone) Fluoxetine (Anti-depressant) Gemfibrozil (Anti-cholesterol)
15 Trace Organic Chemicals Ibuprofen (Analgesic) Meprobamate (Anti-anxiety) Naproxen (Pain-reliever) PFBS (Fluoro-surfactant) PFOA (Fluoro-surfactant) PFOS (Fluoro-surfactant) Primidone (Anticonvulsant) Simazine (Herbicide) Sulfamethoxazole (Antibiotic) TCPP (Flame-retardant) Triclocarban (Anti-microbial) Triclosan (Anti-microbial)
16 Analytical Method Diphenhydramine Atenolol Benzotriazole Caffeine Trimethoprim Primidone Meprobamate Prednisone Simazine Diltiazem TCEP Atrazine Testosterone Naproxen PFOA TCPP Benzophenone Diclofenac Ibuprofen Triclosan Gemfibrozil PFOS Triclocarban DEET
17 True Recoveries in WW Conventional SPE Online SPE Direct Injection Recovery (%) Atenolol d 7 Caffeine C 3 Trimethoprim d 3 Primidone d 5 Meprobamate d 3 Sulfamethoxazole C 6 Diphenhydramine d 5 Ditiazem d 3 Carbamezapine d 10 Dexamethasone d 4 Fluoxetine d 5 TCEP d 12 Atrazine d 5 DEET d 6 Benzophenone d 10 C 1 Naproxen_ Propylparaben d 4 d 3 PFOA C 4 Ibuprofen d 3 PFOS C 4 Gemfibrozil d 6 Triclosan C 12
18 Method Detection Limit 8 replicates using Glaser et al. method 16 8 MDL (ng/l) 4 Concentration (ng/l) Atenolol Atrazine Benzophenone Benzotriazole Bisphenol A Caffeine Carbamezapine Clofibric Acid DEET Diclofenac Diphenhydramine Ditiazem Fluoxetine Gemfibrozil Hydracortisone Hydrochlorothiazide Ibuprofen Meprobamate Naproxen Norgestrel PFHxA PFOA PFOS Primidone Propranolol Propylparaben Simazine Sulfamethoxazole TCEP TCPP Testosterone Triclocarban Triclosan Trimethoprim
19 Matrix Effects SW WWE (1:5 dil) WWE Matrix Effect (%) Atenolol d 7 Atrazine d 5 Benzophenone d 10 Benzotriazole d 4 Bisphenol A C 12 Caffeine C 3 Carbamezapine d 10 DEET d 6 Diclofenac C 6 Diphenhydramine d 5 Ditiazem d 3 Fluoxetine d 5 Gemfibrozil d 6 Ibuprofen d3 Meprobamate d 3 Naproxen C 1 d 3 PFHxA C 2 PFOA C 4 PFOS C 4 Primidone d 5 Propylparaben d 4 Sulfamethoxazole C 6 TCEP d 12 Triclocarban C 6 Triclosan C 12 Trimethoprim d 3 Average
20 Ion Suppression: Online SPE Carbamazepine_d10 Concentration: 100 ppt Injection Vol: 1.5 ml Mass: 150 pg Ultrapure water Wastewater effluent (0.2 um filtered)
21 Ion Suppression: Conventional SPE Carbamazepine_d10 Concentration: 50 ppb Injection Vol: 3 µl Mass: 150 pg Ultrapure water Wastewater effluent (0.2 um filtered)
22 Ion Suppression: Direct Injection Carbamazepine_d10 Concentration: 3 ppb Injection Vol: 50 µl Mass: 150 pg Ultrapure water Wastewater effluent (0.2 um filtered)
23 Ion Suppression Effects Comparison of 3 methods 100 Surrogate Recovery (%) Conventional SPE (500 fold) Online SPE Direct Injection 0 Atenolol d7 Sulfamethoxazole C3 Carbamazepine d10 DEET d6 TCEP d12 Gemfibrozil d6
24 Ion Suppression Effects CSPE OSPE LVI Method Detection Limit (ng/l) Atenolol Meprobamate Sulfamethoxazole Carbamazepine DEET TCEP Gemfibrozil
25 Ion Suppression Effects 1000 CSPE-MRL Method Reporting Limit (ng/l) OSPE-MRL LVI-MRL 0.1 Atenolol Meprobamate Sulfamethoxazole Carbamazepine DEET TCEP Gemfibrozil
26 Analysis of Emerging Contaminants in Water Conventional SPE Method Online SPE Method Direct Injection Method 1 L sample 1.5 ml sample 0.1 ml sample 5 hours 30 min 15 min 36 CECs ng/l 33 CECs ng/ L 21 CECs ng/l
27 Conventional SPE Online SPE Direct Injection Recovery (%) Atenolol d 7 Caffeine C 3 Trimethoprim d 3 Primidone d 5 Meprobamate d 3 Sulfamethoxazole C 6 Diphenhydramine d 5 Ditiazem d 3 Carbamezapine d 10 Dexamethasone d 4 Fluoxetine d 5 TCEP d 12 Atrazine d 5 DEET d 6 Benzophenone d 10 Propylparaben d 4 Naproxen_ C 1 d 3 PFOA C 4 Ibuprofen d 3 PFOS C 4 Gemfibrozil d 6 Triclosan C 12
28 Conclusions q Online SPE allows sensitive analysis of trace organics in water while allowing significant time and labor savings. q Method has been proven to be robust in several different water matrixes. q Online SPE is significantly less affected by ion suppression compared with conventional offline extraction techniques. q LVI is currently not sensitive enough to attain desired MRLs but offers promise with rapid increase in sensitivity of newer mass spectrometers. q Use of online SPE with accurate mass detectors (ToF & Q-ToF) could allow for real-time analysis of trace unknowns in water.
29 Acknowledgements Snyder Research Lab Agilent Technologies Ø Joe Weitzel Ø Dr. Sheher Mohsin
30 Questions Contact:
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