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Journals / Yenilikçi Mühendislik ve Doğa Bilimleri / 2026 / Volume: 5 Issue: 1

Determination of insecticides in honey samples collected from Gümüşhane-Turkiye; Box-Behnken design evaluation of experimental parameters

Erol Erçağ(İSTANBUL ÜNİVERSİTESİ-CERRAHPAŞA)0000-0003-4927-2405
Berrin Saygı Yalçın(YALOVA ÜNİVERSİTESİ)0000-0001-6579-3345
Murat Şahin(TEKİRDAĞ NAMIK KEMAL ÜNİVERSİTESİ)0000-0003-2471-1555
Fehime Jülide Hızal Yücesoy(YALOVA ÜNİVERSİTESİ)0000-0002-5921-0155
Pages
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Publication Date
2025-01-31
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AI Summary & Key Takeaways

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⚡ TL;DR(Too Long; Didn't Read)

Regression analysis showed that the experimental results and the predictive values yielded by model are quite close to each other with determination coefficient (R2) of 0.985.

📌 3 Key Takeaways

🎯
Objective & Hypothesis:This study deals with the investigation of cyfluthrin, cypermethrin, deltamethrin, and malathion residues in local honey samples from Gümüşhane, Turkey.
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Key Findings & Data:The determination was performed with GC/MS-MS method with HP-5MS column under certain conditions: 120 ℃ oven temperature, 250 ℃ injection temperature, 121.9 kPa pressure and 1.2-1.8 mL/min flow rates.
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Conclusion & Impact:Regression analysis showed that the experimental results and the predictive values yielded by model are quite close to each other with determination coefficient (R2) of 0.985.
🔬Design:Modeling & Simulation
📍Scope:Comprehensive Sample
⚙️Variables:Malathion · Deltamethrin · Cypermethrin

Abstract

This study deals with the investigation of cyfluthrin, cypermethrin, deltamethrin, and malathion residues in local honey samples from Gümüşhane, Turkey. The determination was performed with GC/MS-MS method with HP-5MS column under certain conditions: 120 ℃ oven temperature, 250 ℃ injection temperature, 121.9 kPa pressure and 1.2-1.8 mL/min flow rates. The samples were picked from eighteen stations of Gümüşhane. Standard addition method was employed in chromatographic determination. No pesticide detected in samples of fifteen stations, nevertheless, subjected pesticides were determined in samples collected from other three stations. The residue levels varied from 0.18 mg/kg to 9.50 mg/kg at 1.5 mL/min flow rate. The results were also evaluated with Box-Behnken Design (BBD) optimization. Multivariate experimental design (flow rate and station, pesticide type) was employed for constructing quadratic models. Regression analysis showed that the experimental results and the predictive values yielded by model are quite close to each other with determination coefficient (R2) of 0.985.

Özet

This study deals with the investigation of cyfluthrin, cypermethrin, deltamethrin, and malathion residues in local honey samples from Gümüşhane, Turkey. The determination was performed with GC/MS-MS method with HP-5MS column under certain conditions: 120 ℃ oven temperature, 250 ℃ injection temperature, 121.9 kPa pressure and 1.2-1.8 mL/min flow rates. The samples were picked from eighteen stations of Gümüşhane. Standard addition method was employed in chromatographic determination. No pesticide detected in samples of fifteen stations, nevertheless, subjected pesticides were determined in samples collected from other three stations. The residue levels varied from 0.18 mg/kg to 9.50 mg/kg at 1.5 mL/min flow rate. The results were also evaluated with Box-Behnken Design (BBD) optimization. Multivariate experimental design (flow rate and station, pesticide type) was employed for constructing quadratic models. Regression analysis showed that the experimental results and the predictive values yielded by model are quite close to each other with determination coefficient (R2) of 0.985.

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Cite This Article

Erçağ, E., Yalçın, B. S., Şahin, M., Yücesoy, F. J. H. (2025). Determination of insecticides in honey samples collected from Gümüşhane-Turkiye; Box-Behnken design evaluation of experimental parameters. Yenilikçi Mühendislik ve Doğa Bilimleri, Volume: 5 Issue: 1. https://doi.org/10.61112/jiens.1567692

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References (25)

  1. Saleh MA (1980) Mutagenic and carcinogenic effects of pesticides. Journal of Environmental Science and Health Part B 15(6):907–927. https://doi.org/10.1080/03601238009372222
  2. Mukherjee I (2009). Determination of Pesticide Residues in Honey Samples. Bulletin of Environmental Contamination and Toxicology, 83 (6): 818–821. https://doi.org/10.1007/s00128-009-9772-y
  3. Zhang L, Zhao M, Xiao M, Im M-H, Abd El-Aty AM et al (2022) Recent Advances in the Recognition Elements of Sensors to Detect Pyrethroids in Food: A Review. Biosensors, 12:402. https://doi.org/10.3390/bios12060402
  4. El-Osmani R, Net S, Dumoulin D, Bigan M, Ouddane B et al (2014) An experimental design approach to the optimisation of pesticide extraction from water. Anal Methods 6(16):6514-6521. https://doi.org/10.1039/c4ay00610k
  5. Ndungu NN, Kegode TM, Kurgat JK, Baleba SBS, Cheseto X et al (2024) Bio-functional properties and phytochemical composition of selected Apis mellifera honey from Africa. Heliyon 10:e30839. https://doi.org/10.1016/j.heliyon.2024.e30839
  6. Jakkielska D, Frankowski M, Zioła-Frankowska A (2024) Speciation analysis of arsenic in honey using HPLC-ICP-MS and health risk assessment of water-soluble arsenic. Journal of Hazardous Materials 471:134364. https://doi.org/10.1016/j.jhazmat.2024.134364
  7. Sabater C, Calvete I, Vázquez X, Ruiz L, Margolles A (2024) Tracing the origin and authenticity of Spanish PDO honey using metagenomics and machine learning. International Journal of Food Microbiology 421:110789. https://doi.org/10.1016/j.ijfoodmicro.2024.110789
  8. Ek-Huchim JP, Rodríguez-Cab EM, López-Torres E, Dzul-Caamal R, Canepa-Pérez IM et al (2024) Pesticides and polycyclic aromatic hydrocarbons in honey and Apis mellifera from the Yucatán Peninsula, Mexico. Journal of Food Composition and Analysis 132:106293. https://doi.org/10.1016/j.jfca.2024.106293
  9. Wang X, Dong Y, Luan Y, Tian S, Li C et al (2024) Integrated assessment of the spatial distribution, sources, degradation, and human risk of tetracyclines in honey in China. Journal of Hazardous Materials 473:134681. https://doi.org/10.1016/j.jhazmat.2024.134681
  10. Demir E, Recai I (2018) Voltammetric determination of phenmedipham herbicide using a multiwalled carbon nanotube paste electrode. Turkish Journal of Chemistry 42:4. https://doi.org/10.3906/kim-1709-41
  11. Saqaf JM, Soylak M (2021) Supramolecular solvents: a review of a modern innovation in liquid-phase microextraction technique. Turkish Journal of Chemistry 45:6. https://doi.org/10.3906/kim-2110-15
  12. Ostiguy N, Drummond FA, Aronstein K, Eitzer B, Ellis JD et al (2019) Honey Bee Exposure to Pesticides: A Four-Year Nationwide Study. Insects 10:13. https://doi.org/10.3390/insects10010013
  13. Jovanov P, Guzsvány V, Franko M, Lazić S, Sakač M et al (2013) Multi-residue method for determination of selected neonicotinoid insecticides in honey using optimized dispersive liquid–liquid microextraction combined with liquid chromatography-tandem mass spectrometry. Talanta 111:125-133. https://doi.org/10.1016/j.talanta.2013.02.059
  14. Tolcha T, Gemechu T, Al-Hamimi S, Megersa N, Turner C (2020) High density supercritical carbon dioxide for the extraction of pesticide residues in onion with multivariate response surface methodology. Molecules 25(4):1012. https://doi.org/10.3390/molecules25041012
  15. Amvrazi EG, Martini MA, Tsiropoulos NG. (2012). Headspace single-drop microextraction of common pesticide contaminants in honey–method development and comparison with other extraction methods. International Journal of Environmental Analytical Chemistry 92(4):450-465. https://doi.org/10.1080/03067319.2011.585716
  16. Nemati M, Altunay N, Tuzen M, Farajzadeh MA, Afshar Mogaddam MR (2022) In‐situ sorbent formation for the extraction of pesticides from honey. Journal of Separation Science 45(14):2652-2662. https://doi.org/10.1002/jssc.202100963
  17. Tette PAS, Guidi LR, Abreu Glória MB, Fernandes C (2016) Pesticides in honey: A review on chromatographic analytical methods. Talanta 149:124-141. https://doi.org/10.1016/j.talanta.2015.11.045
  18. Briggs GG, Elliott M, Farnham AW, Janes NF, Needham PH et al (1976) Insecticidal activity of the pyrethrins and related compounds VIII. Relation of polarity with activity in pyrethroids. Pesticide Science 7(3):236–240. https://doi.org/10.1002/ps.2780070305
  19. Hamadamin AY, Hassan KI (2020) Gas chromatography-mass spectrometry based sensitive analytical approach to detect and quantify non-polar pesticides accumulated in the fat tissues of domestic animals. Saudi J Biol Sci 27(3):887-893. https://doi.org/10.1016/j.sjbs.2019.12.029
  20. Lu, FC (1995) A Review of the Acceptable Daily Intakes of Pesticides Assessed by WHO. Regulatory Toxicology and Pharmacology 21(3):352-364. https://doi.org/10.1006/rtph.1995.1049
  21. U.S. Environmental Protection Agency. Pesticide Fact Sheet Number 199:Cypermethrin. Office of Pesticides and Toxic Substances, Washington, DC, 1989.2-9.
  22. Pesticide Residues in Food 2000 - Deltamethrin; International Programme on Chemical Safety, Food and Agriculture Organization of the United Nations and World Health Organization: Geneva, Switzerland, 2001; pp 79-110.
  23. Revised Reregistration Eligibility Decision (RED) for Malathion; EPA 738-R-06-030; U.S Environmental Protection Agency, Office of Prevention, Pesticides and Toxic Substances, Office of Pesticide Programs, U.S. Government Printing Office: Washington, DC, 2009.
  24. El-Nahhal Y (2020) Pesticide residues in honey and their potential reproductive toxicity. Science of The Total Environment 741:139953. https://doi.org/10.1016/j.scitotenv.2020.139953
  25. Tolcha T, Gemechu T, Al‐Hamimi S, Megersa N, Turner C (2021) Multivariate optimization of a combined static and dynamic supercritical fluid extraction method for trace analysis of pesticides pollutants in organic honey. Journal of Separation Science 44(8):1716-1726. https://doi.org/10.1002/jssc.202100047