Summary
On-line solid-phase extraction-gas chromatographyion-trap tandem mass spectrometry (SPE-GC-MS/MS) has been used for the trace-level determination of polar and apolar pesticides. The SPE-GC interface, an Autoloop 2000, was operated at an injection temperature of 90°C which permitted the determination of thermolabile pesticides such as carbofuran and carbaryl. Rectilinear calibration curves were obtained for the analytes tested over a range of 0.1–500 ng L−1, using a sample volume of 10–100 mL for enrichment on an SPE cartridge packed with styrene-divinylbenzene copolymer. The detection limits for the pesticides were in the 0.01–4 ng L−1 range. For a number of pesticides acceptable tandem mass spectra were obtained at levels as low as 0.1 ng L−1 level in real-life water samples.
As a demonstration of the applicability of this technique for inorganic anions, bromide and nitrite were converted into 4-bromoacetanilide and 2-phenylphenol, respectively. The reaction products were pooled and subjected to simultaneous analysis by the present method using full-scan mass spectrometric detection. The detection limits were 0.3 and 2 ng L−1, respectively.
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References
D. Barceló, Trends. Anal. Chem.10, 323 (1991).
M. Fielding, D. Barceló, A. Helweg, S. Galassi, L. Tortenson, P. van Zoonen, R. Wolter, G. Angeletti, in “Pesticides in Ground and Drinking Water”, Water Pollution Research Report. No. 27, Commission of the European Community, Brussels, pp. 1–136 (1992).
M.-C. Hennion, V. Pichon, D. Barceló, Trends Anal. Chem.13, 361 (1994).
D. Barceló, M.-C. Hennion, Anal. Chim. Acta318, 1 (1995).
I. Tolosa, J. W. Readman, L. D. Mee, J. Chromatogr. A725, 93 (1996).
The Banning of Halogenated Solvents-Implications for Valid Analytical Measurement. Anal. Proc.30, 321 (1993).
M. W. F. Nielen, R. W. Frei, U. A. Th. Brinkman, in: R. W. Frei and K. Zech (Eds.), “Selective Sample Handling and Detection in High Performance Liquid Chromatography”, Vol.39, Elsevier, Amsterdam (1988).
D. Barceló, Analyst116, 681 (1991).
L. A. Berrueta, B. Gallo, F. Vicente, Chromatographia40, 474 (1995).
A. J. H. Louter, C. A. van Beekvelt, P. Cid Montanes, J. Slobodnik, J. J. Vreuls, U. A. Th. Brinkman, J. Chromatogr. A725, 67 (1996).
K. Grob, “On-line Coupled LC-GC”, Hüthig, Heidelberg (1991).
H.-J. Stan, M. Linkerhägner, J. Chromatogr. A727, 275 (1996).
H. G. J. Mol, M. Althuizen, H.-G. Janssen, C. A. Cramers, U. A. Th. Brinkman, J. High Resol. Chromatogr.19, 69 (1996).
E. Noroozian, F. A. Maris, M. W. F. Nielen, R. W. Frei, G. J. de Jong, U. A. Th. Brinkman, J. High Resol. Chromatogr.10, 17 (1987).
J. J. Vreuls, A. J. H. Louter, U. A. Th. Brinkman, in H.-J. Stan (Ed.), “Chemistry of Plant Protection”, Analysis of Pesticides in Ground and Surface Water, Vol. 12, Part II, Springer-Verlag, Berlin, pp 1–31 (1995).
J. J. Vreuls, R. T. Ghijsen, G. J. de Jong, U. A. Th. Brinkman, J. Chromatogr.625, 237 (1992).
K. Grob, Jr., J. Chromatogr.279, 225 (1983).
K. Grob, B. Schilling, J. Chromatogr.391, 3 (1987).
J. J. Vreuls, A.-J. Bulterman, R. T. Ghijsen, U. A. Th. Brinkman, Analyst117, 1701 (1992).
A. J. H. Louter, U. A. Th. Brinkman, R. T. Ghijsen, J. Microcol. Sep.5, 303 (1993).
Th. M. Noij, M. M. E. van der Kooi, J. High Resol. Chromatogr.18, 535 (1995).
A. J. H. Louter, S. Ramalho, D. Jahr, J. J. Vreuls, U. A. Th. Brinkman, J. Microcol. Sep.8, 469 (1996).
A. Saraf, L. Larsson, J. Mass Spectrom.31, 389 (1996).
A. J. H. Louter, R. Herráez, Hernández, J. J. Vreuls, U. A. Th. Brinkman, Proc. 17th Symp. Capillary Chromatogr., Hüthig, Heidelberg, p. 440 (1995).
S. Schachterle, R. D. Brittain, J. D. Mills, J. Chromatogr. A683, 185 (1994).
E. Grou, V. Radulescu, J. Chromatogr.260, 502 (1983).
G. A. Junk, J. J. Rivhard, Anal. Chem.60, 451 (1988).
E. Ballesteros, M. Gallego, M. Valcarcel, Anal. Chem.65, 1773 (1993).
F. M. Lancas, S. R. Rissato, M. S. Galhiane, J. High Resol. Chromatogr.19, 200 (1996).
K. K. Verma, S. K. Sanghi, A. Jain, D. Gupta, J. Chromatogr.457, 345 (1988).
K. K. Verma, A. Jain, A. Verma, Anal. Chem.64, 1484 (1992).
H.-S. Shin, Y-S. Oh-Shin, J.-H. Kim, J.-K. Ryu, J. Chromatogr. A732, 327 (1996).
A. Jain, A. Chaurasia, B. Sahasrabuddhey, K. K. Verma, J. Chromatogr. A, 1997, in press.
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Verma, K.K., Louter, A.J.H., Jain, A. et al. On-line solid-phase extraction-gas chromatography-ion trap tandem mass spectrometric detection for the nanogram per liter analysis of trace pollutants in aqueous samples. Chromatographia 44, 372–380 (1997). https://doi.org/10.1007/BF02466313
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DOI: https://doi.org/10.1007/BF02466313