The syringyl/guaiacyl ratio was determined for six different Eucalyptus spp. wood clones cultivated in four regions in Brazil. The determinants were made by pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) and the results were compared with those obtained by alkaline nitrobenzene oxidation method. The S/G ratios were obtained considering all the identified lignin derivatives in the pyrograms and also using two groups of markers. The first group of markers consisted of guaiacol, 4-methylguaiacol, 4-vinylguaiacol, trans-isoeugenol, syringol, 4-methylsyringol, 4-vinylsyringol and trans-4-propenylsyringol compounds as markers. The second group included guaiacol, 4-methylguaiacol, 4-vinylguaiacol, vanillin, 4-ethylsyringol, 4-vinylsyringol, syringaldehyde, syringylacetone and trans-4-propenylsyringol. It was observed from the statistical analysis that the values of S/G obtained by Py-GC-MS using the two groups of markers did not differ significantly from those obtained by nitrobenzene oxidation method.

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Recebido em 8/2/08; aceito em 2/9/08; publicado na web em 15/4/09 MATRIX EFFECT IN PESTICIDE QUANTIFICATION BY GAS CHROMATOGRAPHY. The lack of accuracy of a chromatographic method can be associated with the matrix effect. This effect is observed in pesticide quantification by gas chromatography when the chromatographic signals of standards prepared in solvents are compared with those of the analyte in extracts of complex matrices. In the competition between the matrix components and the pesticides for the active sites of the liner, a larger amount of pesticides is transferred to the column, giving apparent extractions above 100%. In this work, we discuss factors that contribute to the matrix effect and present some attempts to overcome the problem.

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Neste trabalho foi avaliado o teor de extrativos em madeiras de eucalipto, por meio de extrações com acetona, mistura de tolueno:etanol (2:1), clorofórmio e diclorometano. As maiores porcentagens de extrativos totais foram obtidas ao utilizar acetona como solvente. Os extratos obtidos em acetona e tolueno:etanol foram ressuspendidos em diclorometano, para avaliação do teor de extrativos lipofílicos. As porcentagens desses extrativos foram semelhantes às obtidas com diclorometano ou clorofórmio, em extrações diretas. Os extratos foram analisados por espectroscopia no infravermelho, para identificação dos principais grupos funcionais dos constituintes extraídos.

In this work, analytical pyrolysis (Py-GC-MS) was employed to identify lignin markers derived from H, S, and G phenylpropanoid units in sugarcane bagasse. Temperatures of 450 and 500 • C allowed the detection of key products that were informative on the bagasse lignin composition. The method was validated by comparing the S/G ratio as determined by the nitrobenzene oxidation (NBO) standard method for five sugarcane varieties. The S/G ratio as determined by Py-GC-MS, taking into consideration all known lignin markers in the analysis, resulted in a correlation coefficient of 0.85 with a linear regression coefficient of 0.74. When a group of selected markers (M2) was used, the correlation coefficient between methods was improved to 0.95 and the linear regression coefficient was adjusted to 0.92. M2 markers consisted of five syringyl markers (syringol, 4-methylsyringol, 4-ethylsyringol, 4-vinylsyringol, and trans-4-propenylsyringol) and four guaiacyl markers (guaiacol, 4-vinylguaiacol, 4-methylguaiacol, and vanillin). Importantly, Py-GC-MS allowed for the study of lignin composition in sugarcane bagasse without the need to remove the extractives, minimizing the work with sample preparations.