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| Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method |
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| DOI： |
| KeyWord:tropical fruits liquid chromatography－quadrupole-time-of-flight mass spectrometry （LC－Q－TOF MS） QuEChERS neonicotinoid insecticides fungicides |
| Author | Institution |
| MEN Xue，WU Xing-qiang，TONG Kai-xuan，XIE Yu-jie，LI Bei，LI Jian-xun，
WEI Jing，WANG Yong-li，FAN Chun-lin，CHEN Hui |
1. Key Laboratory of Food Quality and Safety for State Market Regulation，Chinese Academy of Inspection & Quarantine，Beijing ，China; 2. College of Food Science and Engineering，Shandong Agricultural University，Taian ，China; 3. Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation，Hainan Institute for Food Control，Haikou ，China; 4. Institute of Food Science and Technology，Chinese Academy of Agricultural Sciences，Beijing ，China |
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| Abstract: |
| A liquid chromatography－quadrupole-time-of-flight mass spectrometry（LC－Q－TOF MS） with a modified QuEChERS method was developed for the detection of 33 pesticide residues，including 8 neonicotinoid insecticides and 25 fungicides in four tropical fruits（mango，banana，sweetsop and wax apple）．The pretreatment parameters were optimized by comparing the spiked recoveries obtained with different extraction solvent volumes，buffer salts，and clean-up adsorbent types．Under the optimal experimental conditions，the tropical fruit samples were extracted with 1% acetonitrile acetate in buffer salts（EN salts），and subsequently purified in 15 mL tubes of 900 mg MgSO4，150 mg PSA，50 mg C18 and 15 mg GCB．The sample solutions were detected by LC－Q－TOF MS in positive ion mode under all-ion fragmentation acquisition mode（All Ions MS/MS），and quantified by the matrix-matched external standard method．The method could effectively reduce the matrix effect．Under the optimized conditions，the 33 pesticides showed good linearity in their respective linear ranges，with their correlation coefficients（r2） more than 0.99．The screening detection limits（SDLs） for four tropical fruits were in the range of 0.5－20 μg/kg，and the limits of quantitation（LOQs） were in the range of 0.5－50 μg/kg．The accuracy and precision of the method were verified by the spiked recovery experiments for mangoes．The recoveries for 33 pesticides at three spiked levels ranged from 70.5% to 116%，with relative standard deviations（RSDs） no more than 20%．Meanwhile，the method was successfully applied to the detection of 102 commercial tropical fruits samples．Characterized with simplicity，rapidness and sensitivity，the method was suitable for the detection of neonicotinoid pesticide and fungicide residues in tropical fruits． |
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