Abstract
A headspace solid phase microextraction (HS-SPME) method coupled with gas chromatography and MS detection (GC/MS) was optimized for the simultaneous determination of 21 target Pharmaceuticals and Personal Care Products (PPCPs) in water samples. The analytes included fragrances, UV-filters, antiseptics, estrogens, anti-inflammatory drugs, and pesticides. An on-fiber SPME derivatization, using silyl reagents, was performed for the analysis of more polar acidic compounds. An experimental design approach was applied to systematically investigate and optimize the operative parameters affecting the extraction recovery, namely: extraction temperature and time, derivatization time, desorption temperature and time. The optimum operating conditions were: extraction time of 125 min at a temperature of 40 °C; derivatization time of 30.5 min; desorption time of 2 min at a temperature of 300 °C. Under these conditions, good reproducibility was assessed as RDS% values ≤10% for underivatized PPCPs and ≤20% for derivatized compounds. The method detection limits (LOD) were between 0.7 and 9.0 ng L−1, with the highest values in the range 2.5–9.0 ng L−1 for the derivatized analytes. Method accuracy was evaluated on spiked tap water samples: recoveries varied from 85 to 103% and from 75 to 110% for non-derivatized and derivatized compounds, respectively.
Similar content being viewed by others
References
Daugthon CG, Jones-Lep T, Washington D (2001) Pharmaceuticals and personal care products in the environment: scientific and regulatory issues ACS symposium series American Chemical Society, Washington. Oxford University Press, Washington
Daughton CG (2004) Environ Impact Assess 24:711–732
Loraine GA, Pettigrove ME (2006) Environ Sci Technol 40:687–695
Benotti MJ, Trenholm RA, Vanderford BJ, Holady JC, Stanford BD, Snyder SA (2009) Environ Sci Technol 43:597–603
Dougherty JA, Swarzenski PW, Pinicola RS, Reinhard M (2010) J Environ Qual 49:1173–1180
Brausch JM, Rand GM (2011) Chemosphere 82:1518–1532
U.S. Environmental Protection Agency. Pharmaceuticals and Personal Care Products as Pollutants: http://www.epa.gov/esd/chemistry/ppcp/
Peck AM (2006) Anal Bioanal Chem 386:907–939
Barcelo D, Petrovic M (2007) Anal Bioanal Chem 387:1141–1142
Pietrogrande MC, Basaglia G (2007) Trends Anal Chem 26:1086–1103
Pietrogrande MC, Basaglia G, Dondi F (2009) J Sep Sci 32:1249–1261
Rodil R, Quintana JB, Basaglia G, Pietrogrande MC, Cela R (2010) J Chromatogr A 1217:6428–6435
Rice SL, Mitra S (2007) Anal Chim Acta 589:125–132
Campbell IS, Ton AT, Mulligan CC (2011) J Am Soc Mass Spectrom 22:1285–1293
Pawliszyn J (1997) Solid phase micro extraction: theory and practice. Wiley-VCH Inc, New York
Risticevic S, Niri VH, Vuckovic D, Pawliszyn J (2007) Anal Bioanal Chem 388:1393–1414
Xiangli L, Li L, Shichun Z, Chongyu L, Tiangang L (2006) Chin J Anal Chem 34:325–330
Scheyer A, Morville S, Mirabel P, Millet M (2006) Anal Bioanal Chem 384:475–487
Regueiro J, Llompart M, Garcia-Jares C, Cela R (2009) J Chromatogr A 1216:2816–2824
Fernandez-Alvarez M, Lamas JP, Sanchez-Prado L, Llompart M, Garcia-Jares C, Lores M (2010) J Chromatogr A 1217:6634–6639
Bianchi F, Mattarozzi M, Careri M, Mangia A, Musci M, Grasselli F, Bussolanti S, Basini G (2010) Anal Bioanal Chem 396:2639–2645
Viñas P, Campillo N, Martínez-Castillo N, Hernández-Córdoba M (2010) Anal Bioanal Chem 397:115–125
Basaglia G, Pasti L, Pietrogrande MC (2011) Anal Bioanal Chem 399:2257–2265
Samaras VG, Thomaidis NS, Stasinakis AS, Lekkas TD (2011) Anal Bioanal Chem 399:2549–2561
de Morais P, Stoichev T, Basto MCP, Carvalho PN, Vasconcelos MT (2011) Anal Bioanal Chem 399:2531–2538
Leardi R (2009) Anal Chim Acta 652:161–172
Massart DL, Vandeginste BGM, Deming SN, Michette Y, Kaufman L (1988) Chemometrics: a textbook, Part 2. Elsevier, Amsterdam
Polo M, García-Jares C, Llompart M, Cela R (2007) Anal Bioanal Chem 338:1789–1793
Luan T, Li G, Zhang Z (2000) Anal Chim Acta 424:19–23
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Basaglia, G., Pietrogrande, M.C. Optimization of a SPME/GC/MS Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in Waters. Chromatographia 75, 361–370 (2012). https://doi.org/10.1007/s10337-012-2207-7
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10337-012-2207-7