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Study of Pharmaceuticals in the surface water by GC-MS

Study of Pharmaceuticals in the surface water by GC-MS . Badrinath Dhakal Beatrice Benhamida December-8, 2009. Presentation Outline . Introduction Research Goal Preparation of samples and derivatization Instrumentation and Experimental Procedure

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Study of Pharmaceuticals in the surface water by GC-MS

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  1. Study of Pharmaceuticals in the surface water by GC-MS Badrinath Dhakal Beatrice Benhamida December-8, 2009

  2. Presentation Outline • Introduction • Research Goal • Preparation of samples and derivatization • Instrumentation and Experimental Procedure • Result and discussion • Conclusion • Future Work

  3. Introduction • ~ 3,000 different compounds used in medicines • ~80% or more of the drugs pass through the body unaltered1 • 95 Organic wastewater contaminants (OWCs) in USA2 • Abnormal physiological processes, reproductive impairment, increased incidence of cancer, development of antibiotic-resistant bacteria, potential toxicity of chemical mixture,…

  4. Why is it necessary to analyze pharmaceuticals in water?? • To find the actual information(research value) • To ensure safety of drinking water • Emergency response • To raise awareness and be prepared for the consequences

  5. Methods available • LC-MS: Low sensitivity • HPLC-MS-MS: High sensitivity but expensive and difficult to develop method (EPA method): 74 pharmaceuticals detected till 2007. • GC-MS-MS: High sensitivity but difficult to develop & expensive • GC-MS: Easy to develop, comparatively high sensitivity & cheap.

  6. Research Goal • To identify the acidic pharmaceuticals in the surface water : Acetylsalicylic acid, Ibuprofen and Naproxen • To quantify these pharmaceuticals present in the surface water • To develop a suitable method for the qualitative as well as quantitative analysis of these pharmaceuticals in water

  7. Preparation of samples and standards • Sample water was collected from the Huron River • Filtration of the samples: GlassmicroFiber filter 691 VWR brand • Solid phase extraction: AccuBond SPE ODS-C18 cartridge, Agilent Technologies • Derivatization of the samples : • N,O-bis (trimethylsilyl) trifluoroacetamide (BSTFA)3 • Phenyltrimethylammonium hydroxide(5% in methanol), TCI America

  8. Instrumentation and GC-MS Analysis • Gas chromatography with Mass spectrometer as detector • Varian Chrompack CP-3800 • Varian Saturn 2000 GC/MS • Column 30m long: 5% PDMS, 0.25µm film thickness, 0.25 mm internal diameter • Less-polar stationary phase (strongly-bonded)

  9. Instrumentation &….. • 2 µL sample injected, derivatization at the injection port • EI Auto Scan mode, Range: 40-650, • flow rate: 1.3 ml/min, • Column Oven temp: 70 0c, 10 0 per min up to 250 0 holding for 5 min. • Total time: 25 min. • Stabilization time : 0.25 min

  10. Instrumentation contd…

  11. Result and Discussion

  12. Chromatograms of the standards ibu nap asa

  13. Chromatograms of conc. Std. solution & spiked samples Ibu Nap. ASA

  14. Mass spectra of Ibuprofen

  15. Mass spectra of Naproxen

  16. Chromatograms of Std. solution and Huron river water sample Ibu nap

  17. Conclusion • Only Ibuprofen was detected in the sample water • ASA was not detected in the concentration as high as 100 ppm by this method • Ibuprofen and Naproxen detectable up to 1 ppm. • Use of Internal standard is necessary for the quantitative analysis of these compounds • Appropriate derivatization technique is needed for the trace analysis of these compounds

  18. Future Work • Additional derivatizing agents for these compounds can be explored for the enhancement of trace analysis • New methods of sample preparation, extraction and derivatization can be helpful for the simultaneous analysis of these compounds

  19. References • 1. Togola A.; Budzinski H. , Anal. Bioanal. Chem. (2007) 388:624 • 2. U.S. Geological Survey(1999-2000), Environmental Science and Technology / VOL.36, NO.6,2002 • 3. Budzinski H.; Togola A; Devier MH;Labadie P. Anal. Bioanal. Chem. (2007) 388:624

  20. Acknowledgement • Dr. R.A. Armitage

  21. Thank you!

  22. Questions???

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