Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Published : 2008.12.25

Abstract

A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Keywords

References

  1. Castro, J., Perez, R.A., Sanchez-Brunete, C., Tadeo, J.L. (2001) Analysis of pesticides volatilized from plants and soil by headspace solid-phase microextraction and gas chromatography. Chromatographia Supplement, 53: 361-365. https://doi.org/10.1007/BF02490357
  2. Dugay, J, Miege, C., Hennion, M-C. (1998) Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water. J Chromatography A, 795: 27-42. https://doi.org/10.1016/S0021-9673(97)01036-4
  3. Goncalves, C., Alpendurada M.F. (2002) Comparison of three different poly (dimethylsiloxane)-divinylbenzene fibres for the analysis of pesticide multiresidues in water samples: structure and efficiency. J Chromatography A, 963: 19-26. https://doi.org/10.1016/S0021-9673(02)00645-3
  4. Haib, J., Hofer, I. and Renaud, J.M.(2003) Analysis of multiple pesticide residues in tobacco using pressurized liquid extraction, automated solid-phase extraction clean-up and gas chromatography-tandem mass spectrometry. J. Chromatography A, 1020: 173-187. https://doi.org/10.1016/j.chroma.2003.08.049
  5. Mueller, L., Ward, M.R. (1999), Tobacco, Production, Chemistry and Technology, Davis, D.L., Nielsen, M.T.(Eds.), Blackwell, London, pp. 250-264.
  6. Natnagelo, M., Tabaxzzi, S., Ranelli, R., Benfenati, E. (1999) Analysis of some pesticides in water samples using solid-phase microextraction-gas chromatography with different mass spectrometric techniques. J. Chromatography A, 859: 193-201. https://doi.org/10.1016/S0021-9673(99)00850-X
  7. Shen, J., Xu, X., Cai, J., Shao, X. (2006) Determination of pyrethroid residues in tobacco by means of solid phase microextration and GC/MS with the aid of ultrasonic assisted extraction using water as extracting solvent. Analytical Sciences, 22: 241-244. https://doi.org/10.2116/analsci.22.241
  8. Tahboub, Y.R., Zaater, M.F. and Al-Talla, Z.A. (2005) Determination of the limits of identification and quantitation of selected organochlorine and organophosphorous pesticide residues in surface water by full-scan gas chromatography/mass spectrometry. J. Chromatography A, 1098: 150-155. https://doi.org/10.1016/j.chroma.2005.08.064
  9. Vitali, M., Guidotti, M., Giovinazzo, R., Cedrone, O. (1998) Determination of pesticide residues in wine by SPME and GC/MS for consumer risk assessment. Food Additives and Contaminants, 15: 280-287. https://doi.org/10.1080/02652039809374642