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2014 | 23 | 5 |

Tytuł artykułu

Development and validation of SPE-HPLC-MS/MS method for determining cyclophosphamide in surface waters

Warianty tytułu

Języki publikacji

EN

Abstrakty

EN
A rapid and selective method for trace amounts determination of cyclophosphamide in surface water samples has been developed. A solid phase extraction SPE method for extraction and clean-up procedure has been optimized for determination by reversed-phase high-performance liquid chromatography with tandem mass spectrometry. The analyses proceed in the positive ion mode by means of the electrospray ionization method (ESI). Clean up was accomplished using a polimeric surface modified styrene – divinylobenzene SPE column. The final method was validated according to international chemical harmonization (ICH) standards. High selectivity of assay procedure was obtained by choosing optimal columns (most columns contained a bed modified with C18 groups but varied in the amount of bed: 50-500 mg, and grain size: 33-80 μm) and setting separation conditions, such as flow rate during sorption (2 and 6 mL/min), sorbent type, pH of the sample (samples at pH 3 and 7 were examined), solvent strength during desorption (methanol and dichloromethane), time of evaporation (10, 20, and 30 minutes), type of solvent used for injection (HPLC) (water, methanol and methanol-water mixture, 1:1, v/v), matrix effect (tap water and river water), and time “sample preparationanalysis” on recovery (3, 6, and 9 days). After optimization of sample preparation procedure and analytical conditions environmental water samples were collected from five sampling sites situated in Gdańsk (Pomerania, Poland) and its outskirts and subjected to validated methodology. In four samples cyclophosphamide has been quantified.

Słowa kluczowe

Wydawca

-

Rocznik

Tom

23

Numer

5

Opis fizyczny

p.1537-1545,fig.,ref.

Twórcy

autor
  • Department of Health Sciences, Faculty of Health Sciences with Subfaculty of Nursing and Institute of Maritime and Tropical Medicine, Department of Environmental Toxicology, Medical University of Gdansk, Debowa 23, 80-204 Gdansk, Poland
  • Prolab, Pharmaceutical Analytical Production, Przemyslowa 3, Paterek, 89-100 Nakło n/Notecia, Poland
autor
  • Department of Analytical Chemistry, Chemical Faculty, Gdansk University of Technology (GUT), Narutowicza 11/12 G, 80-952 Gdansk, Poland
autor
  • Department of Analytical Chemistry, Chemical Faculty, Gdansk University of Technology (GUT), Narutowicza 11/12 G, 80-952 Gdansk, Poland

Bibliografia

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  • 2. TERNES T.A. Occurrence of drugs in German sewage treat­ment plants and rivers. Water Res. 32, 3245, 1998.
  • 3. BUERGE I.J., BUSER H.R., POIGER T., MULLER M.D. Occurrence and fate of the cytostatic drugs cyclophos- phamide and ifosfamide in wastewater and surface waters. Environ. Sci. Technol., 40, 7242, 2006.
  • 4. LORAINE G.A., PETTIGROVE M.E. Seasonal variations in concentrations of pharmaceuticals and personal care products in drinking water and reclaimed wastewater in Southern California. Environ. Sci. Technol., 40, 687, 2006.
  • 5. DAUGHTON CH.G., TERNES T.A. Pharmaceuticals and Personal Care Products in the Environment: Agents of Subtle Change?, Environ. Health Persp. 107, Supplement 6, 1999.
  • 6. BAI F., FRAGA CH. H., TAGEN M., SCHAIQUEVICH P., HAGEDORN N., STEWART C.F. Simultaneous determina­tion of cyclophosphamide and carboxyethylphosphoramide mustard in human plasma using online extraction and electrospray tandem mass spectrometry (HTLC-ESI-MS/MS). J. Chromatogr. B, 877, 1709, 2009.
  • 7. STOKVIS E., ROSING H., BEIJNEN J.H. Liquid chro- matography-mass spectrometry for the quantitative bio- analysis of anticancer drugs. Mass Spectrom Rev 24, 887, 2005.
  • 8. VOGESER M, SPOHRER U. Automated processing of whole blood samples for the determination of immunosup- pressants by liquid chromatography tandem-mass spec- trometry. Clin. Chem. Lab. Med., 44, 1126, 2006.
  • 9. CONSTANZER M, CHAVEZ C, MATUSZEWSKI B. Development and comparison of high-performance liquid chromatographic methods with tandem mass spectrometric and ultraviolet absorbance detection for the determination of cyclobenzaprine in human plasma and urine. J Chromatogr B 666, 117, 1995.
  • 10. MAUERER H.H. Current role of liquid chromatogra- phy-mass spectrometry in clinical and forensic toxicology., Anal Bioanal Chem 388, 1315, 2007.
  • 11. ZUCCATO E., CALAMARI D., NATANGELO M., FANELLI R. Presence of therapeutic drugs in the environ­ment, The Lancet, 355, 1789, 2000.
  • 12. TURCI R., SOTTANI C., RONCHI A., MINOIA C. Biological monitoring of hospital personnel occupationally exposed to antineoplastic agents. Toxicol. Lett. 134, 57, 2002.
  • 13. SACHER F., LANGE F.T., BRAUCH H.J., BLANKEN- HORN I. Pharmaceuticals in groundwaters Analytical methods and results of a monitoring program in Baden- Wurttemberg, Germany, J. Chromatogr. A 938, 199, 2001.
  • 14. CASTIGLIONI S., BAGNATI R., CALAMARI D., FANELLI R., ZUCCATO E. A multiresidue analytical method using solid-phase extraction and high-pressure liq­uid chromatography tandem mass spectrometry to measure pharmaceuticals of different therapeutic classes in urban wastewaters, J. Chromatogr. A 1092, 206, 2005.
  • 15. STERGER-HARMANN T., KUMMERER K., SCHAKER J. Trace analisis of antineoplastics isofamide and cyclophos- phamide in sewage water by two step soli phase extraction and GC/MS. J. Chromatogr A, 726, 179, 1996.
  • 16. MOLDOVAN Z. Occurrences of pharmaceutical and per­sonal care products as micropollutants in rivers from Romania. Chemosphere 64, 1808, 2006.
  • 17. CATASTIN C., MULLOT J.U., BOUKARI S., MAZELLI- ER P., LEVI Y., CERVANTES P., ORMSBYA J.N. Assessment of antineoplasic drugs in effluents of two hospi­tals. Eur. J. Water Qual. 39, 171, 2008 [In French].
  • 18. MOLDOVAN Z., CHIRA R., ALDER A.C. Environmental exposure of pharmaceuticals and musk fragrances in the Somes River before and after upgrading the municipal wastewater treatment plant Cluj-Napoca, Romania. Environ. Sci. Pollut. R. 16, (Suppl 1), 46, 2009.
  • 19. MAGNER J. A., ALSBERG T. E., BROMAN D. Bag-SPE - a convenient extraction method for screening of pharma­ceutical residues in influent and effluent water from sewage treatment plants, Anal. Bioanal. Chem., 395, 1481, 2009.
  • 20. YIN J., SHAO B., ZHANG J., LI K. A Preliminary Study on the Occurrence of Cytostatic Drugs in Hospital Effluents in Beijing, China. B. Environ. Contam. Tox. 2009.
  • 21. KONIECZKA P., NAMIEŚNIK J. Assessment and control of chemical analyses data, WNT Warsaw, 2007 [In Polish].
  • 22. PAWLACZYK J., ZAJĄC M. Validation of chemical analy­sis method, A.M. Poznań, 2001 [In Polish].
  • 23. Validation of an analytical method - Polfa seminar materi­als, Book 9, Warsaw 1995 [In Polish].
  • 24. Commission of the European Communities. The rules gov­erning medicinal products in the European community, vol III Addendum. Note for guidance; analytical validation July 1989/Luxemburg: The Commission, 1990.

Typ dokumentu

Bibliografia

Identyfikatory

Identyfikator YADDA

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