Abstract:
Fresh egg samples were shelled, thoroughly homogenized, and uniformly mixed. An aliquot (5 g) was taken, to which 10 mL of acetonitrile, 4 mg of anhydrous magnesium sulfate, and 1 g of sodium chloride were added, followed by vortex oscillation for 20 min and centrifugation for 3 min. A portion (5 mL) of the supernatant was taken, to which 200 mg of C
18, 600 mg of
N-propyl ethylenediamine (PSA), 10 mg of graphitized carbon black (GCB), and 800 mg of anhydrous magnesium sulfate were added, followed by vortex oscillation for 20 min and centrifugation for 3 min. The supernatant was passed through a 0.22 μm organic filter membrane, and the filtrate was analyzed by ultra-high performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry. In the chromatographic analysis, Shim-pack XR-ODS Ⅱ C
18 column was used as the stationary phase, with acetonitrile-water system as the mobile phase for gradient elution. In the mass spectrometric analysis, electrospray ionization (ESI) source was used in positive and negative ion modes, with multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode for detection. A standard mass spectrometry library containing information such as characteristic daughter ions and their abundance was constructed to aid in qualitative analysis, and matrix matched external standard method was used for quantification. It was shown that linear relationships between the mass concentrations and peak areas of quantitative ions were kept in the ranges of 1.0−100 μg·L
−1 (dinotefuran, flufenoxuron, cyclaniliprole, and flubenzimine) and 0.50−50 μg·L
−1 (the other target compounds), with detection limits in the range of 0.500−5.00 μg·kg
−1. Spike recovery tests at three concentration levels were made on blank samples, giving recoveries in the range of 71.9%−119%, and RSDs (
n=6) of the determined values ranged from 1.3% to 14%. The proposed method was applied to the analysis of 90 batches of actual samples, and flubendiamide, hexaflumuron, teflubenzuron, and cyclaniliprole were simultaneously detected in 1 batch of samples with detection amounts of 24.3, 12.6, 9.54, 25.8 μg·kg
−1, matching degrees of which with the standard mass spectrometry library were 73.532%, 85.659%, 78.168%, 93.822%, respectively.