A simple, specific, and rapid analytical method for determining seven largely used carbamate insecticides in tomato, spinach, lettuce, zucchini, pear, and apple is here presented. This method is based on the matrix solid-phase dispersion technique, with heated water as extractant followed by liquid chromatography (LC)-mass spectrometry (MS) equipped with a single quadrupole and an electrospray ion source. Target compounds were extracted from the vegetal matrixes by water heated at 50 degreesC. After acidification and filtration, 0.25 mL of any aqueous extract was injected in the LC column. MS data acquisition was performed in the selected ion monitoring mode, selecting three ions for each target compound. Heated water appeared to be an excellent extractant because recovery data ranged between 76 (carbaryl in spinach) and 99% (pirimicarb in spinach), with RSDs not larger than 10%. Using trimethacarb (an obsolete carbamate insecticide) as a surrogate internal standard, the accuracy of the analysis varied between 84 and 110%, with RSDs not larger than 9%. On the basis of a signal-to-noise ratio of 10, limits of quantification were estimated to range between 2 (pirimicarb) and 10 ppb (oxamyl) and were not influenced by the type of matrix. When trying to fractionate analytes by using a short chromatographic run time, marked weakening of the ion signals for oxamyl, methomyl, and aldicarb were observed. This effect was traced to polar endogenous co-extractives eluted in the first part of the chromatographic run that interfered with gas-phase ion formation for carbamates. Adopting more selective chromatographic conditions eliminated this effect.

A simple and rapid assay for analyzing residues of carbamate insecticides in vegetables and fruits: hot water extraction followed by liquid chromatography-mass spectrometry / Bogialli, Sara; Curini, Roberta; DI CORCIA, Antonio; Nazzari, Manuela; D., Tamburro. - In: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY. - ISSN 0021-8561. - STAMPA. - 52:4(2004), pp. 665-671. [10.1021/jf035195j]

A simple and rapid assay for analyzing residues of carbamate insecticides in vegetables and fruits: hot water extraction followed by liquid chromatography-mass spectrometry

BOGIALLI, Sara;CURINI, Roberta;DI CORCIA, Antonio;NAZZARI, Manuela;
2004

Abstract

A simple, specific, and rapid analytical method for determining seven largely used carbamate insecticides in tomato, spinach, lettuce, zucchini, pear, and apple is here presented. This method is based on the matrix solid-phase dispersion technique, with heated water as extractant followed by liquid chromatography (LC)-mass spectrometry (MS) equipped with a single quadrupole and an electrospray ion source. Target compounds were extracted from the vegetal matrixes by water heated at 50 degreesC. After acidification and filtration, 0.25 mL of any aqueous extract was injected in the LC column. MS data acquisition was performed in the selected ion monitoring mode, selecting three ions for each target compound. Heated water appeared to be an excellent extractant because recovery data ranged between 76 (carbaryl in spinach) and 99% (pirimicarb in spinach), with RSDs not larger than 10%. Using trimethacarb (an obsolete carbamate insecticide) as a surrogate internal standard, the accuracy of the analysis varied between 84 and 110%, with RSDs not larger than 9%. On the basis of a signal-to-noise ratio of 10, limits of quantification were estimated to range between 2 (pirimicarb) and 10 ppb (oxamyl) and were not influenced by the type of matrix. When trying to fractionate analytes by using a short chromatographic run time, marked weakening of the ion signals for oxamyl, methomyl, and aldicarb were observed. This effect was traced to polar endogenous co-extractives eluted in the first part of the chromatographic run that interfered with gas-phase ion formation for carbamates. Adopting more selective chromatographic conditions eliminated this effect.
2004
CARBAMATES; HOT WATER EXTRACTION; HPLC-MS/MS
01 Pubblicazione su rivista::01a Articolo in rivista
A simple and rapid assay for analyzing residues of carbamate insecticides in vegetables and fruits: hot water extraction followed by liquid chromatography-mass spectrometry / Bogialli, Sara; Curini, Roberta; DI CORCIA, Antonio; Nazzari, Manuela; D., Tamburro. - In: JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY. - ISSN 0021-8561. - STAMPA. - 52:4(2004), pp. 665-671. [10.1021/jf035195j]
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11573/359866
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