250
hydroalcoholic solution and the fiber coating the selection of the coating necessarily
entailed a compromise between the amount of extracted analytes and reproducibility. The best working conditions were obtained by using the 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane coating and 5% ethanol. The experimental
variables affecting the SPME were optimized using a CCD. Extraction time, extraction temperature, and percentage of sodium chloride were selected as the most critical factors. The outcomes of the optimization procedure indicate that the maximum
value was achieved by setting the extraction time 45 min, extraction temperature
80 °C, and NaCl percentage 10% (w:w). In particular it was observed a substantial
improvement in terms of precision at 80 °C which could be due to the depletion of
the ethanol from the aqueous solution.
The assay of the analytes was performed by using tandem mass spectrometry in
selected reaction monitoring (SRM) acquisition mode. The proposed method was
carefully validated in terms of linearity, accuracy, precision (intra- and interday) and
limit of quantification.
The method was applied to a real case scenario by analyzing PM10 samples collected at the monitoring station of the CNR-IIA in Rende. The results showed the
presence of some of the investigated pollutants at a concentration above the lower
limit of quantification of the method. These findings can be due to the closeness of
the sampling area to the industrial area of Cosenza and the motorway, which crosses
the area at about 1 Km east of the measurements site.
23.3 Conclusions
We set-up a new approach for the determination of the toxic chemicals from solid
matrices. We base the analytical strategy on an MAE extraction of the analytes from
the solid matrix using an eco-friendly hydroalcoholic mixture followed by the analysis using suitable instrumental equipment. Compared to the protocols generally
used, which mainly use Soxhlet as extraction technique, the developed approach
does not provide for the use of damaging organic solvents, is faster and automatable. As a case study, we presented the new approach through the analysis of OPEs
from particulate matter. The final protocol reached satisfactory values in terms of
linearity, sensitivity, lower limit of quantification, matrix effect, accuracy, and
precision.
References
1. Camel V (2000) TrAC – trends anal. Chem 19:229–248
2. Sanchez-Prado L, Garcia-Jares C, Llompart M (2010) J Chromatogr A 1217:2390–2414
3. Naccarato A, Gionfriddo E, Elliani R, Pawliszyn J, Sindona G, Tagarelli A (2018) J Sep Sci
41:929–939
4. Cavaliere B, Monteleone M, Naccarato A, Sindona G, Tagarelli A (2012) J Chromatogr
A. 1257:149–157
A. Naccarato et al.
hydroalcoholic solution and the fiber coating the selection of the coating necessarily
entailed a compromise between the amount of extracted analytes and reproducibility. The best working conditions were obtained by using the 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane coating and 5% ethanol. The experimental
variables affecting the SPME were optimized using a CCD. Extraction time, extraction temperature, and percentage of sodium chloride were selected as the most critical factors. The outcomes of the optimization procedure indicate that the maximum
value was achieved by setting the extraction time 45 min, extraction temperature
80 °C, and NaCl percentage 10% (w:w). In particular it was observed a substantial
improvement in terms of precision at 80 °C which could be due to the depletion of
the ethanol from the aqueous solution.
The assay of the analytes was performed by using tandem mass spectrometry in
selected reaction monitoring (SRM) acquisition mode. The proposed method was
carefully validated in terms of linearity, accuracy, precision (intra- and interday) and
limit of quantification.
The method was applied to a real case scenario by analyzing PM10 samples collected at the monitoring station of the CNR-IIA in Rende. The results showed the
presence of some of the investigated pollutants at a concentration above the lower
limit of quantification of the method. These findings can be due to the closeness of
the sampling area to the industrial area of Cosenza and the motorway, which crosses
the area at about 1 Km east of the measurements site.
23.3 Conclusions
We set-up a new approach for the determination of the toxic chemicals from solid
matrices. We base the analytical strategy on an MAE extraction of the analytes from
the solid matrix using an eco-friendly hydroalcoholic mixture followed by the analysis using suitable instrumental equipment. Compared to the protocols generally
used, which mainly use Soxhlet as extraction technique, the developed approach
does not provide for the use of damaging organic solvents, is faster and automatable. As a case study, we presented the new approach through the analysis of OPEs
from particulate matter. The final protocol reached satisfactory values in terms of
linearity, sensitivity, lower limit of quantification, matrix effect, accuracy, and
precision.
References
1. Camel V (2000) TrAC – trends anal. Chem 19:229–248
2. Sanchez-Prado L, Garcia-Jares C, Llompart M (2010) J Chromatogr A 1217:2390–2414
3. Naccarato A, Gionfriddo E, Elliani R, Pawliszyn J, Sindona G, Tagarelli A (2018) J Sep Sci
41:929–939
4. Cavaliere B, Monteleone M, Naccarato A, Sindona G, Tagarelli A (2012) J Chromatogr
A. 1257:149–157
A. Naccarato et al.