Determination of 15 high-risk pesticide and adjuvant residues in fruits from USA by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry
Received:February 14, 2019    Download the full
DOI：10.16801/j.issn.1008-7303.2019.0060
Key Words:solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  imported fruits  high-risk pesticides  adjuvant  maximum residue limit (MRL)
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Author NameAffiliationE-mail
LAN Feng Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LI Xiaoliang Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
DUAN Xiaona Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
JIANG Wei Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
ZANG Hongwei Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LIU Chuande Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
ZHOU Xianxue Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
LU Zeqi Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China  
WANG Zhixin Laboratory of Quality and Safety Risk Assessment for Fruit(Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China 343684502@163.com 
HUA Zeke Agricultural Technology Promotion Center of Laiyang, Laiyang 265200, Shandong Province, China  
WANG Tianyi Agricultural Technology Promotion Center of Laiyang, Laiyang 265200, Shandong Province, China  
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Abstract:
      A method was developed for the quantative determination of 15 high-risk pesticide and adjuvant (acephate, methomyl, thiamethoxam, thiabendazole, acetamiprid,simazine, pyrimethanil, fludioxonil, boscalid, methoxyfenozide, myclobutanil, fenhexamid, tetraconazole, piperonyl butoxide, chlorpyrifos) residues by SPE-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The samples were homogenized, extracted with acetonitrile, and cleaned-up by amino solid phase extraction column. The separation was performed on a Shimadu Shim-pack XR-ODS column (75 mm×2.0 mm, 1.6 μm). The compounds were identified by MS/MS and multiple reaction monitoring (MRM) mode, and quantified by external standard method. The linearities of 15 pesticides and adjuvants were in the concentration range of 0.001-0.5 mg/L, with the correlation coeffecients higher than 0.999 5. At the fortified levels from 0.005 mg/kg to 0.5 mg/kg in pear, grape and apple, the average recoveries of all 15 pesticides and adjuvants ranged from 80% to 115% with the relative standard deviations varied from 5.5% to 16%. The limits of quantification (LOQs) of the analytes were ranged from 0.005 to 0.01 mg/kg. This method is simple, rapid, accutate and therefore, suitable for the confirmation and quantification of the 15 pesticides and adjuvants in fruits.
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