Screening of 258 Pesticide Residues in Silage Using Modified QuEChERS with Liquid- and Gas Chromatography-Quadrupole/Orbitrap Mass Spectrometry
Yujie Xie,
Xingqiang Wu,
Yanling Song,
Yini Sun,
Kaixuan Tong,
Xiaoxuan Yu,
Chunlin Fan,
Hui Chen
Affiliations
Yujie Xie
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
Xingqiang Wu
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
Yanling Song
Laboratory of Heilongjiang Feihe Dairy Co., Ltd., Qiqihar 164800, China
Yini Sun
Laboratory of Heilongjiang Feihe Dairy Co., Ltd., Qiqihar 164800, China
Kaixuan Tong
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
Xiaoxuan Yu
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
Chunlin Fan
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
Hui Chen
Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection & Quarantine, No. 11, Ronghua South Road, Beijing 100176, China
A method for the simultaneous screening of 258 pesticide residues in silage using modified QuEChERS combined with liquid chromatography (LC)- and gas chromatography (GC)- quadrupole-Orbitrap mass spectrometry (Q-Orbitrap/MS) has been developed. After hydration, the silage was homogenized with a 1% acetic acid–acetonitrile solution, and the extract was purified using C18, PSA, and anhydrous magnesium sulfate. Finally, the sample was detected using LC/GC-Q-Orbitrap/MS, and quantified using an external standard method. The results showed that 258 pesticides had an excellent linear relationship in the range of 0.1–50 μg L−1, and that the coefficients of determination (R2) were more than 0.99. The screening detection limit (SDL) of silage was in the range of 0.5–50 μg kg−1, and the limit of quantitation (LOQ) was in the range of 1–50 μg kg−1. The accuracy and precision of the method were verified at the spiked levels of 1-, 2- and 10-times LOQ, and the recovery of 258 pesticides was in the range of 66.5–119.8%, with relative standard deviations (RSDs) of less than 20% (n = 6). This method was simple, rapid, and reliable, and could be applied to screen and quantify multi-pesticide residues in silage.
