Overall calibration procedure via a statistically based matrix-comprehensive approach in the stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry analysis of pesticide residues in fruit-based soft drinks.
Stir bar sorptive extraction (SBSE)-thermal desorption (TD) procedure combined with gas chromatography mass spectrometry (GC-MS) and the statistical variance component model (VCM) is applied to the determination of semi-volatile compounds including organochlorine and organophosphorus pesticides in various synthetic and real fruit-based soft drink matrices. When the matrix effects are corrected using isotopically labelled or non labelled internal standard, but matrix/calibration run-induced deviations are still present in the measurements, the adoption of a variance component model (VCM) in the quantitative analysis of various matrices via an overall calibration curve is successful. The method produces an overall calibration straight line for any analyte accounting for the uncertainty due to all the sources of uncertainty, namely matrix-induced deviations, calibration runs performed at different times, measurement errors. Small increases in the detection limits and in uncertainty in the concentration values obtained in the inverse regression face favourably the decrease in times and costs for routine analyses.
Department of Chemical Sciences, University of Padova, Padova, Italy.
Irma
I
Lavagnini
Alessandro
A
Urbani
Franco
F
Magno
D001628:Beverages; D002138:Calibration / Q000592:standards; D003627:Data Interpretation, Statistical; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D008962:Models, Theoretical; D010573:Pesticide Residues / Q000737:chemistry*; D013696:Temperature
D010573:Pesticide Residues