Food Analytical Methods

, Volume 12, Issue 1, pp 176–189 | Cite as

Multi-residue Analysis of 34 Pesticides in Black Pepper by QuEChERS with d-SPE Vs. d-SLE Cleanup

  • Wei Yao
  • Zihao Zhang
  • Shuangyu Song
  • Xianghong Hao
  • Yanjun Xu
  • Lijun HanEmail author


In this study, quick, easy, cheap, effective, rugged, and safe (QuEChERS) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was applied and optimized in determination of 34 commonly used pesticides in black pepper. Two cleanup approaches including dispersive solid-phase extraction (d-SPE) and dispersive solid liquid extraction (d-SLE) were investigated and compared. The results showed that for d-SPE method, 26 target pesticides met the analytical recovery and RSD requirements (recoveries 60–120%, RSDs 2–28%) and LODs were 0.5–1 μg/kg, while for d-SLE method, 19 target pesticides met the analytical requirements (recoveries 60–117%, RSDs 3–24%) and the LODs were 0.5–2.5 μg/kg. Cleanup by d-SLE showed lower matrix effects and lower sensitivity due to the dilution factor, while d-SPE method could be applicable to more pesticides due to better sensitivity. It was therefore decided that d-SPE cleanup would be used in the final method for multi-residue analysis in black pepper. The method was developed and validated to determine the residues of 34 pesticides in 15 black pepper market samples collected from 11 different provinces in China. Four pesticides were detected, including clothianidin (0.02 mg/kg) that was detected in one sample and acetamiprid (< LOQ to 0.07 mg/kg) in seven samples, both were lower than their MRLs, but the residue of carbendazim in seven samples and metalaxyl-M in two samples excessed their MRLs (0.1 mg/kg) established by EU.


Black pepper Pesticides QuEChERS d-SPE d-SLE 



This study was funded by the China National Keynote Research & Development Plan (grant number 2017YFD0800700).

Compliance with Ethical Standards

Conflict of Interest

Wei Yao declares that he has no conflict of interest. Zihao Zhang declares that she has no conflict of interest. Shuangyu Song declares that she has no conflict of interest. Xianghong Hao declares that she has no conflict of interest. Yanjun Xu declares that he has no conflict of interest. Lijun Han 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, LLC, part of Springer Nature 2018

Authors and Affiliations

  • Wei Yao
    • 1
  • Zihao Zhang
    • 1
  • Shuangyu Song
    • 1
  • Xianghong Hao
    • 1
  • Yanjun Xu
    • 1
  • Lijun Han
    • 1
    Email author
  1. 1.College of ScienceChina Agricultural UniversityBeijingChina

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