Direkt Daldırma Katı Faz Mikroekstraksiyon Yöntemi İle Kiraz Örneklerinde Klorpirifos Kalıntılarının Gaz Kromatografisi Kütle Spektrometresinde Tayini

Year 2018, Volume: 30 Issue: 4, 398 - 402, 31.12.2018

Oya Aydın Urucu , Ece Kök Yetimoğlu , Deniz Devecioğlu

https://doi.org/10.7240/marufbd.398657

Cited By: 1

Abstract

A method based on a solid phase
microextraction gas chromatography- mass spectrometry (SPME-GC/MS) was
developed for the quantitative determination of chlorpyrifos residues in cherry
samples. Three kinds of fiber coatings: PA (polyacrylate, 85µm), PDMS–DVB
(polydimethylsiloxane–divinylbenzene 65 mm) and PDMS (polydimethylsiloxane, 100
mm) were compared. Various parameters affecting SPME procedures such as
temperature, extraction and desorption times, salinity, stirring rate were
investigated. The analytes from all sample extracts were preconcentrated for 30
minutes in the SPME fiber at 60 °C and then the fiber was desorbed by heating
at 250 °C for 10 minutes in the gas chromatography injection port. Limits of
detection (LOD) and quantitation (LOQ) values were 0.03 µg/L and 0,1 µg/L,
respectively. An average recovery range was 93-98% with relative standard
deviation (RSD) < 10 %.

Keywords

Fiber, Pesticides, Sample handing

Determination of Chlorpyrifos Residues in Cherry Samples by Direct Immersion Solid Phase Microextraction Coupled with Gas Chromatography Mass Spectrometry

Abstract

A method based on a solid phase
microextraction gas chromatography- mass spectrometry (SPME-GC/MS) was
developed for the quantitative determination of chlorpyrifos residues in cherry
samples. Three kinds of fiber coatings: PA (polyacrylate, 85µm), PDMS–DVB
(polydimethylsiloxane–divinylbenzene 65 mm) and PDMS (polydimethylsiloxane, 100
mm) were compared. Various parameters affecting SPME procedures such as
temperature, extraction and desorption times, salinity, stirring rate were
investigated. The analytes from all sample extracts were preconcentrated for 30
minutes in the SPME fiber at 60 °C and then the fiber was desorbed by heating
at 250 °C for 10 minutes in the gas chromatography injection port. Limits of
detection (LOD) and quantitation (LOQ) values were 0.03 µg/L and 0,1 µg/L,
respectively. An average recovery range was 93-98% with relative standard
deviation (RSD) < 10 %.

Keywords

Fiber, Pesticides, Sample handing

References

• [1] Buchel, K. H. (1983) Chemistry of Pesticides, Hardcover, 42-70.[2] Gündüz, Z. Y. (2013) Determination of pesticides in gas chromatography with solid phase microextraction method. PhD thesis, Marmara University FBE, Istanbul, Turkey, 15-30.[3] Zhang, L., Liu, S., Cui, X., Pan, C., Zhang, A. and Chen, F. (2012) A review of sample preparation methods for the pesticide residue analysis in foods. Cent. Eur. J. Chem., 10(3), 900-925.[4] Ho, Y. M., Tsoi Y. K. and Sze-Yin, K. L. (2013) Highly sensitive and selective organophosphate screening in twelve commodities of fruits, vegetables and herbal medicines by dispersive liquid–liquid microextraction, Analytical Chimica Acta, 58(775), 58-66.[5] Andreu, V. and Pico, Y., (2004) Determination of pesticides and their degradation products in soil: critical review and comparison of methods, Trends in Analytical Chemistry 23 (10), 772-789.[6] Cardoso, A. S., Feliciano, S.A. and Rebelo, M. H. (2009) Optimization and validation of a SPME-GC-ECD methodology for the determination of organochlorine pesticides in natural spring waters from portugalthe. Journal of Society of Ecological Chemistry and Engineering 16 (52), 138.[7] Coelho, E., Ferreira, C. and Almeida, M. M. C. J. (2008) Analysis of Polynuclear Aromatic Hydrocarbons by SPME-GC-FID in Environmental and Tap Waters Braz. Chem. Soc. 19, 1084-1097.[8] Ma, J., Xiao, R., Li, J., Zhao, X., Shi, B. and Li, S. (2009) Determination of organophosphorus pesticides in underground water by SPE-GC-MS. J Chromatogr Sci. 47 110-115.[9] Popiel S. and Sankowska, M. (2011) Determination of chemical warfare agents and related compounds in environmental samples by solid-phase microextraction with gas chromatography. Journal of chromatography A (1218) 8457-8479.[10] Pawliszyn, J. (1999) Applications of solid phase microextraction, The Royal Society of Chemistry, Cambridge, UK, 57-7.