Food Analytical Methods

, Volume 10, Issue 6, pp 1826–1843 | Cite as

Determination of 103 Pesticides and Their Main Metabolites in Animal Origin Food by QuEChERS and Liquid Chromatography–Tandem Mass Spectrometry



A rapid and sensitive analytical multiresidue method has been developed for the simultaneous determination of 103 pesticides (herbicides, insecticides, and fungicides) and 18 metabolites in foods of animal origin using liquid chromatography-tandem with triple quadrupole in dynamic multiple reaction monitoring (DMRM) mode. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation technique was established, and the efficiency of the dispersive solid-phase extraction (d-SPE) cleanup step was evaluated by comparing the effects of different d-SPE sorbent combinations (primary secondary amine (PSA) + graphitized carbon black (GCB), PSA + C18, C18, and C18 + GCB). The limits of quantification (LOQs) ranged from 1 to 10 μg/kg, and the coefficient of determination (R 2) was ≥0.995 within the calibration linearity range of 0–250 μg/L for all pesticides. The combination of C18 + GCB was validated at two spiking levels (10 and 50 μg/kg) in chicken, fish, pork, and rabbit. Satisfactory recoveries (70–119%) and RSDs ≤17% were achieved for all analytes, except for naptalam (60–69%), pyrimethanil (40–49%), and thiabendazole (62–66%) at 10 μg/kg spiking level. The validated method was successfully applied to the analysis of real samples of food of animal origin.


Animal origin foods Pesticide residues Metabolites QuEChERS LC-MS/MS 


Compliance with Ethical Standards


This work has been carried out with support from the Public Welfare Fund of Inspection and Quarantine of China (201410177), the National Key Research and Development Program of China (2016YFD0401105), and the Shrimp and Crab Innovation Team of Shandong Agriculture Research System of China (SDAIT-13-07).

Conflict of Interest

Huili Zhang declares that she has no conflict of interest. Jianhua Wang declares that he has no conflict of interest. Li Li declares that she has no conflict of interest. Ying wang declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.


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Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  1. 1.Ocean University of ChinaQingdaoChina
  2. 2.Technical Center of Inspection and QuarantineShandong Entry-Exit Inspection and Quarantine BureauQingdaoChina
  3. 3.Chinese Academy of Inspection and Quarantine BureauBeijingChina
  4. 4.Marine Biology Institute of Shandong ProvinceQingdaoChina

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