Abstract:
The citrus juice sample (10.00 g) was taken and placed in a 50 mL-centrifuge tube, and 20.0 mL of acetonitrile was added. The mixture was shaken well and vortex extracted for 3 min. An extraction salt package (containing 6 g of magnesium sulfate anhydrous and 1.5 g of sodium chloride) was added, and the mixture was shaken, cooled down and centrifuged for 3 min. The supernatant was drawn using a 2 mL syringe solid phase extraction cartridge (containing 25 mg of
N-propylethylenediamine, 2.5 mg of graphitized carbon black, 150 mg of magnesium sulfate anhydrous, and connecting with a 0.22 μm organic phase filter membrane), in which the residues of 12 carbamate pesticides, including aldicarb sulfoxide, aldicarb sulfone, methomyl, 3-hydroxycarbofuran, aldicarb, metolcarb, propoxur, carbofuran, carbaryl, isoprocarb, dimethacarb and fenobucarb were determined by high performance liquid chromatography-tandem mass spectrometry. Agilent ZORBAX Eclipse Plus C
18 chromatographic column was used as the stationary phase and the mixed solution composed of methanol and 5 mmol · L
−1 ammonium acetate solution containing 0.1% (volume fraction) formic acid at different volume ratios was used as the mobile phase for gradient elution. Electrospray ion (ESI) source was used for mass spectrometry. The targets were analyzed by multiple reaction monitoring (MRM) mode in positive ion (ESI
+) scanning mode, and matrix matching method was used for quantitative analysis. As shown by the results, linear relationships between the corresponding response intensities of quantitative ions and mass concentrations of 12 carbamate pesticides were kept in the range of 0.5-10.0 μg · L
−1, with lower limits of determination (10S/N) of 1.0 μg · kg
−1. Test for recovery was made by the standard addition method, giving results in the range of 86.8%-104%, with RSDs (
n=6) of the determined values in the range of 1.2%-7.5%. This method was used for analysis of 30 actual citrus juice samples, and carbofuran was detected in 2 samples, with detection amounts of 1.6 and 4.2 μg · kg
−1, respectively.