Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry |
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Authors: | Liu Xingang Xu Jun Dong Fengshou Li Yuanbo Song Wenchen Zheng Yongquan |
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Institution: | (1) Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, 100193, China;(2) Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing, 100125, China; |
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Abstract: | The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination
of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography
coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and
halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary
secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds
was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide,
and halofenozide and in negative mode (ESI−) for chromafenozide. The limits of detection were below 0.6 μg kg−1, while the limit of quantification did not exceed 2 μg kg−1 in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory
recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and
1 mg kg−1). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged
from 74.2% to 112.5% with RSDs in the range of 1.4–13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical
method for diacylhydrazine insecticide in vegetables and fruits. |
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