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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
Article

Abstract

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.

Keywords

Black pepper Pesticides QuEChERS d-SPE d-SLE 

Notes

Funding

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.

References

  1. Abou-Arab AAK, Abou Donia MA (2001) Pesticide residues in some Egyptian spices and medicinal plants as affected by processing. Food Chem 72(4):439–445CrossRefGoogle Scholar
  2. Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast easy multiresidue method employing acetonitrile extraction/partitioning, “dispersive soild-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 86(2):412–431Google Scholar
  3. Barker SA (2007) Matrix soild phase dispersion (MSPD). J Biochem Biophys Methods 70(2):151–162CrossRefGoogle Scholar
  4. Chai LK, Elie F (2013) A rapid multi-residue method for pesticide residues determination in white and black pepper (Piper nigrum L.). Food Control 32(1):322–326CrossRefGoogle Scholar
  5. Cheng C, Di SS, Zhang WJ, Chen L, Tian ZN, Zhou ZQ, Diao JL (2018) Determination of cyanamide residue in 21 plant-derived foods by liquid chromatography-tandem mass spectrometry. Food Chem 239:529–534CrossRefGoogle Scholar
  6. Chiarello M, Graeff RN, Minetto L, Cemin G, Schneider VE, Moura S (2017) Determination of pesticides in water and sediment by HPLC-HRMS and its relationship with the use and land occupation. Quim Nova 40(2):158–165Google Scholar
  7. Codex Alimentarius Commission (CAC) guideline CAC/GL 90-2017 (2017) Guidelines on performance criteria for methods of analysis for the determination of pesticide residues in food and feedGoogle Scholar
  8. Da Luz SFM, Yamaguchi LF, Kato MJ, de LOF, Xavier LP, Maia JGS, de R. Ramos A, Setzer WN, da Silva JKdR (2017) Secondary metabolic profiles of two cultivars of piper nigrum (black pepper) resulting from infection by fusarium solani f. sp. piperis. Int J Mol Sci 18(12):2434–2451CrossRefGoogle Scholar
  9. Daulatabad CD, Mulla GM, Mirajkar AM (1995) Vernolic and cyclopropenoic fatty acids in piper nigrum seed oil. Eur J Lipid Sci Technol 97(12):453–454Google Scholar
  10. Gorgani L, Mohammadi M, Najafpour GD, Nikzad M (2017) Piperine-the bioactive compound of black pepper: from isolation to medicinal formulations. Compr Rev Food Sci F 16(1):124–140CrossRefGoogle Scholar
  11. Han XW, Kang D, Zhang HZ, Lu P, Hu DY (2016) Dinotefuran residue in paddy soil, brown rice, rice hull and rice plant determined by modified QuEChERS/LC-MS/MS. Guizhou Agr Sci 44(5):47–50Google Scholar
  12. He YH, Wang L, Wang J (2017) Determination of 15 pesticide residues in food matrixes by ultra performance liquid chromatography tandem mass spectrometry after sample cleanup using polyethersulfone (PES)/multiwalled carbon nanotubes (MWCNTs) composite membrane. Food Sci 38(18):317–324Google Scholar
  13. Hou X, Lei SR, Qiu ST, Guo LA, Yi SG, Liu W (2014) A multi-residue method for the determination of pesticides in tea using multi-walled carbon nanotubes as a dispersive solid phase extraction absorbent. Food Chem 153(24):121–129CrossRefGoogle Scholar
  14. Kolberg DI, Prestes OD, Adaime MB, Zanella R (2011) Development of a fast multiresidue method for the determination of pesticides in dry samples (wheat grains, flour and bran) using QuEChERS based method and GC-MS. Food Chem 125(4):1436–1442CrossRefGoogle Scholar
  15. Lehotay SJ, De Kok A, Hiemstra M, van Bodegraven P (2005) Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J AOAC Int 88(2):595–614Google Scholar
  16. Lehotay SJ, Mastovska K, Lightfield AR, Gates RA (2010) Multi-analyst, multi-matrix performance of the QuEChERS approach for pesticide residues in foods and feeds using HPLC/MS/MS analysis with different calibration techniques. J AOAC Int 93(2):355–367Google Scholar
  17. Lozowicka B, Rutkowska E, Jankowska M (2017) Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD. Environ Sci Pollut Res Int 24(8):7124–7138CrossRefGoogle Scholar
  18. Ponce-Robles L, Rivas G, Esteban B, Oller I, Malato S, Aguera A (2017) Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem 409(26):6181–6193CrossRefGoogle Scholar
  19. Qiu J, Zhang LS, Song WC, Yang SM, Dai SH, Xue XH (2010) Simultaneous determination of chloroacetanilide herbicide residues in crops with gas chromatography-mass spectrometry. Der Pharma Chem 2(6):349–357Google Scholar
  20. Rahman MM, Abd El-Aty AM, Kim SW, Shin SC, Shin HC, Shim JH (2017) Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: a review. J Sep Sci 40(1):203–212CrossRefGoogle Scholar
  21. Ramyashreedevi GS, Singh D, Srivastava A, Biswas KK, Gupta AK (2017) Characterization of Xanthomonas species causing bacterial leaf spot disease of pepper (Capsicum annuum) in India. India J Arg Sci 87(12):1679–1686Google Scholar
  22. Srivastava LP, Budhwar R, Raizada RB (2001) Organochlorine pesticide residues in Indian spices. J Sci Food Agric 67(6):856–862Google Scholar
  23. Sun Q, Wang WM, Li YB, Wen GY, Tang HX, Song WG, Dong MF (2017) A novel approach for simultaneous determination E/Z-fluoxastrobins in vegetables and fruits by UHPLC-DAD. Food Control 78:7–13CrossRefGoogle Scholar
  24. Valverde S, Ares AM, Bernal JL, Nozal MJ, Bernal J (2018) Effect of the storage conditions (light and temperature) on the detection of thiamethoxam and clothianidin content in rapeseeds by LC-DAD. Food Anal Methods 11(1):161–169CrossRefGoogle Scholar
  25. Wu NC, Zhang Q, Liu CH, Le Y, Li PP, Li SH, Li CL (2016) Determination of chlorpyrifos and deltamethrin residues in white pepper by combined gel permeation chromatography and solid phase extraction with gas chromatography-tandem mass spectrometry. Pesticide 12(55):903–905Google Scholar
  26. Yogendrarajah P, Van Poucke C, De Meulenaer B, De Saeger S (2013) Development and validation of a QuEChERS based liquid chromatography tandem mass spectrometry method for the determination of multiple mycotoxins in spices. J Chromatogr A 1297(13):1–11CrossRefGoogle Scholar
  27. Zhang ZH, Feng MY, Zhu KC, Han LJ, Sapozhnikova Y, Lehotay SJ (2016) Multiresidue analysis of pesticides in straw roughage by liquid chromatography-tandem mass spectrometry. J Agric Food Chem 64(31):6091–6099CrossRefGoogle Scholar
  28. Zheng WQ, Yang JF, Yu H, Li ZG, Zu C, Wang C, Sang LW, Liu AQ (2017) Present status and Iinnovation development of black pepper industry in China. China J Tro Agr 37(12):102–108Google Scholar
  29. Zhu F, Mojel R, Li GT (2018) Physico chemical properties of black pepper (Piper nigrum) starch. Carbohydr Polym 181:986–993CrossRefGoogle Scholar

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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