Abstract
A headspace solid phase microextraction coupled to gas chromatography with electron capture detector (HS-SPME-GC-ECD) method was optimized for the determination of seven chlorophenols (CPs) with different levels of chlorination. This is the first time that HS-SPME-GC-ECD with acetylation of the analytes is used for the simultaneous determination of CPs in water samples. The influence of fibre type, derivatization conditions, salt addition, temperature and time of extraction and temperature of desorption was checked. Possible sources of contamination and analyte losses were considered. The best results were obtained with the polydimethylsiloxane/divinylbenzene fibre, derivatization by acetylation using 100 μL of acetic anhydride and 0.1 g of anhydrous sodium carbonate per 10 mL of sample, salt addition of 100 g L−1 sodium chloride, extraction at 70 °C for 60 min and desorption in the GC injector at 260 °C for 6 min. The limits of detection (LOD) for monochlorophenols were 12 and 122 ng L−1 for 2-chlorophenol and 4-chlorophenol, respectively. For polychlorinated CPs, the LODs were lower than 6 ng L−1, values similar to the existing methods that use SPME with derivatization for CPs determination in water samples. The method is suitable for the determination of CPs in most environmental aqueous samples. Repeatability and reproducibility were less than 16.8% and 11.7%, respectively. The optimized method was successfully applied for the analysis of waters with complex matrices such as river and estuarine water samples.
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References
Michalowicz J, Duda W (2007) Polish J of Environ Stud 16:347–362
Morales S, Canosa P, Rodríguez I, Rubí E, Cela R (2005) J Chromatogr A 1082:128–135
Quintana JB, Rodil R, Muniategui-Lorenzo S, López-Mahía P, Prada-Rodríguez D (2007) J Chromatogr A 1174:27–39
Bagheri H, Saraji M (2001) J Chromatogr A 910:87–93
Li J, Zhao X, Shi Y, Cai Y, Mou S, Jiang G (2008) J Chromatogr A 1180:24–31
Bagheri H, Saber A, Mousavi SR (2004) J Chromatogr A 1046:27–33
Basher C, Lee HK (2004) J Chromatogr A 1057:163–169
Fattahi N, Assadi Y, Hosseini MRM, Jahromi EZ (2007) J Chromatogr A 1157:23–29
Fattahi N, Samadi S, Assadi Y, Hosseini MRM (2007) J Chromatogr A 1169:63–69
Llompart M, Lourido M, Landín P, García-Jares C, Cela R (2002) J Chromatogr A 963:137–148
Limam I, Guenne A, Driss MR, Mazéas L (2010) Inter J Environ Anal Chem 90:230–244
Canosa P, Rodriguez I, Rubí E, Cela R (2005) J Chromatogr A 1072:107–115
Lee M-R, Yeh Y-C, Hsiang W-S, Hwang B-H (1998) J Chromatogr A 806:317–324
Simões NG, Cardoso VV, Ferreira E, Benoliel MJ, Almeida CMM (2007) Chemosphere 68:501–510
Wei M-C, Jen J-F (2002) Chromatographia 55:701–706
Silva SL, Alves A, Santos L (2009) J Chromatogr Sci 47:1–7
Bianchi F, Careri M, Mucchino C, Musci M (2002) Chromatographia 55:595–606
Insa S, Salvadó V, Anticó E (2004) J Chromatogr A 1047:15–20
Martínez-Uruñuela A, González-Sáiz JM, Pizarro C (2004) J Chromatogr A 1048:141–151
Guillard RRL (1975) Culture of phytoplankton for feeding marine invertebrates. In: Smith WL, Chanley MH (eds) Culture of marine invertebrates animals. Plenum, New York
Mani V (1999) Properties of commercial SPME coatings. In: Pawliszyn J (ed) Applications of solid phase microextraction. The Royal Society of Chemistry, Cambridge
Grote C, Levsen K (1999) The application of SPME in water analysis. In: Pawliszyn J (ed) Applications of solid phase microextraction. The Royal Society of Chemistry, Cambridge
Yang K-W, Eisert R, Lord H, Pawliszyn J (1999) Determination of pesticides in foods by automated SPME-GC-MS. In: Pawliszyn J (ed) Applications of solid phase microextraction. The Royal Society of Chemistry, Cambridge
Matich AJ (1999) Analysis of food and plant volatiles. In: Pawliszyn J (ed) Applications of solid phase microextraction. The Royal Society of Chemistry, Cambridge
Ai J (1999) Quantitation by SPME before reaching the partition equilibrium. In: Pawliszyn J (ed) Applications of solid phase microextraction. The Royal Society of Chemistry, Cambridge
Lee J, Khalilian F, Bagheri H, Lee HK (2009) J Chromatogr A 1216:7678–7693
Acknowledgements
This work was partially funded by Fundação para a Ciência e a Tecnologia (FCT), Portugal, through fellowships awarded to P. de Morais (SFRH/BD/66492/2009), T. Stoichev (SFRH/BPD/32700/2006) and P. Carvalho (SFRH/BD/44934/2008), co-financed by POPH/FSE and the REEQ/304/QUI/2005 re-equipment project.
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de Morais, P., Stoichev, T., Basto, M.C.P. et al. A headspace SPME-GC-ECD method suitable for determination of chlorophenols in water samples. Anal Bioanal Chem 399, 2531–2538 (2011). https://doi.org/10.1007/s00216-010-4610-y
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DOI: https://doi.org/10.1007/s00216-010-4610-y