Citation: PAN Xiao-Bo, YI Xiong-Hai, SHI Yi-Yin, ZHAO Shan-Zhen, SHENG Yong-Gang, DENG Xiao-Jun, ZHU Jian, DING Zhuo-Ping. Rapid Screening and Confirmation of Residue Compounds in Foods from Regulation of Pesticides in HongKong by Liquid Chromatography Coupled with High Resolution Quadrupole Time-of-Flight Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(7): 1125-1132. doi: 10.11895/j.issn.0253-3820.150917 shu

Rapid Screening and Confirmation of Residue Compounds in Foods from Regulation of Pesticides in HongKong by Liquid Chromatography Coupled with High Resolution Quadrupole Time-of-Flight Mass Spectrometry

1.
College of Food Science, Shanghai Ocean University, Shanghai 201306, China;
2.
Shanghai Exit-Entry Inspection and Quarantine Bureau, Shanghai 200135, China

Received Date: 16 November 2015
Revised Date: 4 March 2016

A method for screening of 249 residue compounds of pesticide in foods from the Hongkong's regulation was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS). The target analytes were dissolved in acetonitrile with 1% formic acid, then extracted and purified by using a modified QuEChERS method. The chromatographic separation was performed on an Agilent Poroshell 120 EC-C₁₈ column (150 mm×3 mm i.d., 2.7 μm) with gradient elution using 0.1% (V/V) formic acid and methanol as mobile phase. The target compounds were monitored under positive ionization mode with ESI source. The matrix effects in 11 kinds of typical foods were considered and the quantification was carried out by matrix-matched with external standard method. Two databases of accurate mass and fragment ions were created. The results demonstrated that the linear range was from 10 μg/kg to 500 μg/kg with good correlation coefficients (r>0.90). The method quantitation limits were in the range of 10-100 μg/kg (S/N≥10). For rices, mushrooms, soybeans, spinaches, tomatoes, broccolies, grapefruits, chives, carrots, lettuces and cucumbers, the average recoveries at three spiked levels were in the range of 23.2%-133.2%, 35.6%-137.6%, and 38.7%-140.2%, and the relative standard deviations (RSDs) were 1.3%-19.2% (n=6). The method is simple, time-saving with high sensitivity and good reproducibility, as well as having practical application for its low test cost.
- Liquid chromatography coupled with quadrupole time-of-flight mass spectrometry,
- Pesticide,
- Screening
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沈阳化工大学材料科学与工程学院沈阳 110142