Improved analysis of 230 pesticide residues in three fermented soy products by using automated one-step accelerated solvent extraction coupled with GC-MS/MS.

ABSTRACT

Consumer concerns over healthy diets are increasing as a result of the toxicity and persistence of pesticide residues in foodstuffs. Developing sensitive and high-throughput monitoring techniques for these trace residues is seen as an essential step in ensuring food safety. An automatic and sensitive multi-residue analytical method was developed and validated for the simultaneous determination of 230 compounds, including pesticides and their hazardous metabolites, in fermented soy products. The method included preparing the sample using on-line extraction and clean-up system based on accelerated solvent extraction (ASE), then determining the analytes using GC-MS/MS techniques. The homogenized samples (soy sauce, douchi, and sufu) were automatically extracted at 80 °C and 10.3 MPa and at the same time, in situ cleaned by 300 mg of primary secondary amine (PSA) combined with 20 mg of hydroxylated multi-walled carbon nanotubes in an extraction cell. The method obtained excellent calibration linearity (r > 0.9220) and a satisfactory analysis of the targeted compounds, which were evaluated with matrix-matched calibration standards over the range of 5-500 µg L-1. The limit of detections (LODs) of analytes were in the range of 0.01-1.29 µg kg-1, 0.01-1.39 µg kg-1, and 0.01-1.34 µg kg-1 in soy sauce, douchi, and sufu, respectively. The limit of quantifications (LOQs), which defined as the lowest spiking level, were set at 5.0 µg kg-1. The recoveries were within 70-120 % for over 95 % of the analytes, and the relative standard deviations (RSDs) were below 13.6 %. Moreover, a positive detection rate of 47 % were obtained when the proposed method was used on 15 real fermented soy products. These results suggested that the developed high-throughput method is highly feasible for monitoring of these target analytes in trace level.