Validation of Pesticides Multi-Residual Testing Method on Nutmeg by Using UPLC-MS/MS

Bayu Refindra Fitriadi*    -  Balai Besar Perbenihan dan Proteksi Tanaman Perkebunan Surabaya, Indonesia

(*) Corresponding Author

The use of pesticides in nutmeg still leaves an accumulation of pesticide residues that can endanger human health and damage the ecological balance. In addition, nutmeg with high pesticide residue content will be rejected by nutmeg export destination countries. This research was conducted to validate the method of testing pesticide residues of carbaryl, carbofuran, acetate, and dimethoate on nutmeg. This pesticide residue test uses the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) optimization method and is analyzed using UPLC-MS/MS (Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry). This method meets the validation requirements according to SANTE/12682/2019. The limit of quantification (LOQ) of the analyte is below the Maximum Residue Limit (MRL) set by the European Union through Regulation (EC) No. 396/2005. 

Keywords: Pesticide residue; UPLC-MS/MS; nutmeg; QuEChERS

  1. Anastassiades. M. et al. (2003) ‘Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce’. Journal of AOAC International. 86. pp. 412–431. DOI: 10.1093/jaoac/86.2.412
  2. Badan Standardisasi Nasional. (2017) SNI ISO/IEC 17025:2017 Persyaratan umum kompetensi laboratorium pengujian dan laboratorium kalibrasi. Jakarta: Badan Standardisasi Nasional.
  3. Biziuk. M. and Stocka. J. (2015) ‘Multiresidue Methods for Determination of Currently Used Pesticides in Fruits and Vegetables Using QuEChERS Technique’. International Journal of Environmental Science and Development. 6(1). pp. 18-22. DOI: 10.7763/IJESD.2015.V6.554
  4. Boes. E. et al. (2015) ‘Development of validated method using QuEChERS technique for organochlorine pesticide residues in vegetable’. Procedia Chemistry. 16. 229–236. https://doi.org/10.1016/j.proche.2015.12.052
  5. Boneva. I.. Yaneva. S.. and Danalev. D. (2021) ‘Development and validation of method for determination of organophosphorus pesticides traces in liver sample by GC-MS/MS-ion trap’. Acta Chromatographica. 33(2). pp. 188–194. DOI: https://doi.org/10.1556/1326.2020.00778
  6. British Standard. (2018) ‘Foods of Plant Origin. Multimethod for the Determination of Pesticide Residues Using GC- and LC-Based Analysis Following Acetonitrile Extraction/partitioning and Clean-up by Dispersive SPE. Modular QuEChERS-method (BS EN 15662:2018)’. BSI: Brussels.
  7. Chawla. S. et al.. (2017) ‘Evaluation of Matrix Effects in Multiresidue Analysis of Pesticide Residues in Vegetables and Spices by LC-MS/MS’. Journal of AOAC International. 100(3). pp. 616-623. DOI: 10.5740/jaoacint.17-0048
  8. Das. S. et al. (2020) ‘Validation of a Multiresidue Method for the Analysis of 86 Multiclass Pesticides in Litchi Fruit by Gas Chromatography–Tandem Mass Spectrometry’. Journal of AOAC International. 103(1). hal. 46-54. https://doi.org/10.5740/jaoacint.19-0203
  9. Dinar. L.. Suyantohadi. A.. dan Fajar. M.A. (2013) ‘Kajian Standar Nasional Indonesia Biji Pala’. Jurnal Standardisasi. 15(2). 83 - 90. DOI: http://dx.doi.org/10.31153/js.v15i2.111
  10. Direktorat Jenderal Perkebunan. (2019) ‘Statistik Perkebunan Indonesia. Pala’. Jakarta: Direktorat Jenderal Perkebunan Kementerian Pertanian.
  11. Dutta. D.. Hingmire. S.. Banerjee. K. (2020) ‘Multiresidue Analysis of Pesticides in Moringa Pods by GC-MS/MS and LC-MS/MS’. Journal of AOAC International. 103(6). pp. 1486–1497. DOI: 10.1093/jaoacint/qsaa053
  12. Ekaputri. R.A. (2013) ‘Validasi Analisis Residu Pestisida Karbaril. Klorpirifos. dan Dimetoat dalam Buah Menggunakan Metode QuEChERS dan LC-MS/MS’. Skripsi. Jakarta: Universitas Indonesia.
  13. Eurachem. (1998) ‘The fitness for purpose of analytical method: A laboratory guide to method validation and related topics.’ Diakses tanggal 19 Maret 2021 dari: https://www.eurachem.org/images/stories/Guides/pdf/MV_guide_1998_EN.pdf
  14. Ferronato. G. et al. (2018) ‘Determination of organochlorine pesticides (OCPs) in breast milk from Rio Grande do Sul. Brazil. using a modified QuEChERS method and gas chromatography-negative chemical ionisation-mass spectrometry’. International Journal of Environmental Analytical Chemistry. 98(11). 1005–1016. DOI: 10.1080/03067319.2018.1518441
  15. Fitriadi. B.R.. dan Putri. A.C. (2016) ‘Penentuan Residu Pestisida Deltametrin dan λ-Sihalotrin pada Lada (Piper nigrum L.) Menggunakan Metode QuEChERS’. Indo. J. Chem. Sci.. 5(2). hal. 91-97. DOI 10.15294/IJCS.V5I2.8908
  16. Fitriadi. B.R.. dan Putri. A.C. (2019) ‘Dampak Aplikasi Pestisida Sipermetrin. Deltametrin. Klorpirifos dan λ-Sihalotrin Terhadap Kandungan Residu Pestisida pada Biji Kakao’. Jurnal Agrosains dan Teknologi.3(2). hal. 10-18. DOI: https://doi.org/10.24853/jat.4.1.10-18
  17. Harmoko. Kartasasmita. R.E.. and Tresnawati. A. (2015) ‘QuEChERS Method for the Determination of Pesticide Residues in Indonesian Green Coffee Beans using Liquid Chromatography Tandem Mass Spectrometry’. J. Math. Fund. Sci.. 47(3). pp. 296-308. https://doi.org/10.5614/j.math.fund.sci.2015.47.3.7
  18. Jahanmard. E.. Ansari. F.. and Feizi. M. (2016) ‘Evaluation of QuEChERS sample preparation and GC mass spectrometry method for the determination of 15 pesticide residues in tomatoes used in salad production plants’. Iranian Journal of Public Health. 45(2). pp. 230–238.
  19. Koçyiğit. H. and Sinanoğlu. F. (2020) ‘Method validation for the analysis of pesticide residue in aqueous environment’. Environ Monit Assess. 192:567. pp. 1-13 DOI: 10.1007/s10661-020-08523-8
  20. Machado. I.. et al. (2017) ‘Determination of pesticide residues in globe artichoke leaves and fruitsby GC–MS and LC–MS/MS using the same QuEChERS procedure’. Food Chemistry. 227. pp. 227– 236. DOI: 10.1016/j.foodchem.2017.01.025
  21. Mancha A.. and Fuentes J. (2008). Evaluation of the health beneficial properties of the aromatic ether Myristicin. a volatile oil derived from various plants sources. The University of Texas-Pan American 1201 W. University Drive Edinburg. Texas. diakses tanggal 22 September 2021 dari http://agrilifecdn.tamu.edu/phytochemicals/files/2011/03/Myristicin_Nov9_330PM.ppt
  22. Mastovska. K.. and Lehotay. S.J.. 2004. ‘Evaluation of Common Organic Solvents for Gas Chromatographic Analysis and Stability of Multiclass Pesticide Residues’. Journal of Chromatography A. 1040: 259–272. doi: 10.1016/j.chroma.2004.04.017.
  23. Paz. M. et al. (2017) ‘Application of the QuEChERS method for the determination of organochlorine pesticide residues in Brazilian fruit pulps by GC-ECD’. J of Environmental Science and Health. Part B. 52(1). pp. 48–58. https://doi.org/10.1080/03601234.2016.1229450
  24. Pesireron. M. et al. (2019) ‘Perbaikan Teknik Pengendalian Hama dan Penyakit pada Perkebunan Pala Banda (Myristica Fragrants Houtt) di Maluku’. Jurnal Littri. 25(1). hal. 45 - 58. DOI: http://dx.doi.org/10.21082/littri.v25n1.2019.45-58
  25. SANTE. (2019) ‘SANTE/12682/2019 Analytical Quality Control and Method Validation Procedures for Pesticide Residues Analysis in Food and Feed’. Diakses tanggal 9 Maret 2021 dari https://www.eurl-pesticides.eu/userfiles/file/EurlALL/AqcGuidance_SANTE_2019_12682.pdf.
  26. SANTE. (2020) SANTE/2020/12830 ‘Guidance Document on Pesticide Analytical Methods for Risk Assessment and Post-approval Control and Monitoring Purposes’. Diakses tanggal 19 September 2021 dari https://ec.europa.eu/food/system/files/2021-02/pesticides_mrl_guidelines_2020-12830.pdf.
  27. Zhang. Y. et al. (2016) ‘Multiresidue determination of pyrethroid pesticide residues in pepper through a modified QuEChERS method and gas chromatography with electron capture detection’. Biomed. Chromatogr.. 30. pp. 142-148. https://doi.org/10.1002/bmc.3528

Open Access Copyright (c) 2021 Walisongo Journal of Chemistry
Creative Commons License
This work is licensed under a Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License.

WJC: Walisongo Journal of Chemistry
Published by the Department of Chemistry
Faculty of Science and Technology
Universitas Islam Negeri Walisongo Semarang
Jl Prof. Dr. Hamka Kampus II Ngaliyan Semarang 50185
Phone: +62 857-4272-8650
Website: https://fst.walisongo.ac.id/
Email: wjc@walisongo.ac.id

ISSN: 2549-385X (Print)
ISSN: 2621-5985 (Online)

apps