Bìa tạp chí

Website: https://vjfc.nifc.gov.vn/

009bet

Study on production of reference material for plant protection chemicals: bifenthrin, carbofuran, chlorpyrifos, difenoconazole, imidacloprid in milk powder matrix

Nguyen Thi Thu Ha Pham Van Khue Luu Thi Huyen Trang Do Thi Thu Hang Pham Thi Huong Giang Pham Hoang Thi Nguyen Hoang Anh Pham Nhu Trong Nguyen Thi Thanh Thuy Nguyen Thi Anh Huong Nguyen Thi Minh Hoa
Received: 29 Sep 2025
Revised: 01 Jan 1900
Accepted: 01 Jan 1900
Published: 29 Sep 2025

Article Details

How to Cite
Nguyen Thi Thu Ha, Pham Van Khue, Luu Thi Huyen Trang, Do Thi Thu Hang, Pham Thi Huong Giang, Pham Hoang Thi, Nguyen Hoang Anh, Pham Nhu Trong, Nguyen Thi Thanh Thuy, Nguyen Thi Anh Huong, Nguyen Thi Minh Hoa. "Study on production of reference material for plant protection chemicals: bifenthrin, carbofuran, chlorpyrifos, difenoconazole, imidacloprid in milk powder matrix". Vietnam Journal of Food Control. vol. 8, no. 3, pp. 158-168, 2025
PP
158-168
Counter
3

Main Article Content

Abstract

Controlling pesticide residues in food is a top concern to ensure consumer health and safety. In testing, reference materials (RM) and certified reference materials (CRM) are essential tools used to calibrate equipment, control quality and confirm the reliability of analytical methods. This study focuses on the production, storage and evaluation of certified reference materials of five pesticides: bifenthrin, carbofuran, chlorpyrifos, difenoconazole, imidacloprid in powdered milk, in compliance with international standards ISO 17034:2016 and ISO 33405:2024. The RM after production and packaging were analyzed by gas chromatography (GC) (for bifenthrin and chlorpyrifos) and liquid chromatography (LC) (for carbofuran, difenoconazole and imidacloprid) using tandem mass spectrometry detector (MS/MS) to evaluate homogeneity, stability and estimate shelf life. The results showed that at room temperature, the RM was estimated to be stable with all five pesticides for at least 2 years. The RM after evaluation was used to successfully organize a proficiency testing program with the participation of 07 testing laboratories nationwide. The certified value is accompanied by the expanded measurement uncertainty of each pesticide: difenoconazole 77.90 ± 10.35 µg/kg; carbofuran 81.55 ± 10.02 µg/kg; bifenthrin 68.38 ± 8.47 µg/kg; imidacloprid 65.15 ± 8.22 µg/kg; chlorpyrifos 69.04 ± 13.97 µg/kg.

Keywords:

Bifenthrin, carbofuran, clorpyrifos, difenoconazole, imidacloprid, reference material, milk powder.

References

[1]. K. L. Bassil, C. Vakil, M. Sanborn, D. C. Cole, J. S. Kaur, and K. J. Kerr, "Cancer health effects of pesticides," Canadian Family Physician, vol. 53, no. 10, pp. 1704–1711, 2007.
[2]. Ministry of Health, "50/2016/TT-BYT, Maximum Limits On Residues Of Pesticide In Food," 2016 (in Vietnamese) [Online]. Available https://thuvienphapluat.vn/van-ban/The-thao-Y-te/Thong-tu-50-2016-TT-BYT-gioi-han-toi-da-du-luong-thuoc-bao-ve-thuc-vat-trong-thuc-pham-337490.aspx.
[3]. Marcella Vitoria Galindo et al., "Comprehensive analysis of contaminants in Brazilian infant formulas: Application of QuEChERS coupled with UHPLC-QqQ-MS/MS and suspect screening-unknown analysis by UHPLC-Q-Orbitrap-MS," Journal of Chromatography A, vol. 1726, 464967, 2024.
[4]. Vandana Tripathy et al., "Monitoring and dietary risk assessment of pesticide residues in brinjal, capsicum, tomato, and cucurbits grown in Northern and Western regions of India," Journal of Food Composition and Analysis, vol. 110, 104543, 2022.
[5]. M. M. Gómez-Ramos, C. Ferrer, O. Malato, A. Agüera, and A. R. Fernández-Alba, "Liquid chromatography-high-resolution mass spectrometry for pesticide residue analysis in fruit and vegetables: Screening and quantitative studies," Journal of Chromatography A, vol. 1287, pp. 24–37, 2013.
[6]. H. V. Botitsi, S. D. Garbis, A. Economou, and D. F. Tsipi, "Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices," Mass Spectrometry Reviews , vol. 30, no. 5, pp. 907–939, 2011.
[7]. K. Pszczolińska and M. Michel, "The QuEChERS Approach for the Determination of Pesticide Residues in Soil Samples: An Overview,” Journal of AOAC International, vol. 99, no. 6, pp. 1403–1414, 2016.
[8]. AOAC Official Method 2007.01, "Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate,” 2007.
[9]. TCVN 9333:2012, "Foods - Determination of pescitides residue by gas chromatography mass spectrometry and liquid chromatography tandem mass spectrometry - QuEChERS method,” 2012 (in Vietnamese). [Online]. Available https://thuvienphapluat.vn/tcvn/cong-nghe-thuc-pham/tcvn-9333-2012-thuc-pham-xac-dinh-du-luong-thuoc-bao-ve-thuc-vat-phuong-phap-912767.aspx.
[10]. TCVN 8245:2009, "Reference materials – General and statistical principles for certification,” 2009 (in Vietnamese). [Online]. Available: https://thuvienphapluat.vn/TCVN/Linh-vuc-khac/TCVN-8245-2009-mau-chuan-Nguyen-tac-chung-nguyen-tac-thong-ke-trong-chung-nhan-908063.aspx.
[11]. T. Yarita et al., "Development of soybean certified reference material for pesticide residue analysis," Talanta, vol. 119, pp. 255–261, 2014.
[12]. T. Otake et al., "Development of green onion and cabbage certified reference materials for quantification of organophosphorus and pyrethroid pesticides," Journal of Agricultural and Food Chemistry, vol. 59, no. 16, pp. 8568–8574, 2011.
[13]. T. Otake et al., "Development of certified reference material for quantification of two pesticides in brown rice," Journal of Agricultural and Food Chemistry, vol. 57, no. 18, pp. 8208–8212, 2009.
[14]. J. K. Quirijns, K. G. Van Der Paauw, E. J. Mulders, and B. Griepink, "Development of Milk Powder Reference Materials BCR-CRM 187,188. Part I. Preparation, Homogeneity, and Stability," Journal of Analytical chemistry and microbiology, vol. 73, no. 5, pp. 773–776, 1990.
[15]. Y. Chen et al., "Preparation of a reference material for tea containing five pesticide residues and its evaluation in an interlaboratory comparison study in China," Accreditation and Quality Assurance, vol. 27, no. 2, pp. 93–101, 2022.
[16]. T. Otake et al., "Development of apple certified reference material for quantification of organophosphorus and pyrethroid pesticides," Food Chemistry, vol. 138, no. 2–3, pp. 1243–1249, 2013.
[17]. F. Zhao, J. Liu, B. Han, and J. Luo, "Investigation and Validation of Detection of Storage Stability of Difenoconazole Residue in Mango," Journal of Food Quality, vol. 2019, no. 1, 5641643, 2019.
[18]. Y. Liu, X. Qin, Q. Chen, Q. Zhang, P. Yin, and Y. Guo, "Effects of moisture and temperature on pesticide stability in corn flour," Journal of the Serbian Chemical Society, vol. 85, no. 2, pp. 191–201, 2020.
[19]. ISO 33405:2024 Reference materials — Approaches for characterization and assessment of homogeneity and stability, Ed. 1, 2024.
[20]. ISO/IEC 17043:2023 Conformity assessment — General requirements for the competence of proficiency testing providers, Ed. 2, 2023.
[21]. ISO/IEC 17025:2017 General Requirements for the competence of testing and calibration laboratories, 2017.
[22]. CEN Method 15662 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, European Standard, 2018.
[23]. ISO 33405:2024 Reference materials — Approaches for characterization and assessment of homogeneity and stability, Ed. 1, 2024.
[24]. [24]. ISO 17034:2016 General requirements for the competence of reference material producers, Ed. 1, 2016.
[25]. ISO 5725-2:2019 Accuracy (trueness and precision) of measurement methods and results. Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method, Ed. 2, 2019.
[26]. ISO 13528:2015 Statistical methods for use in proficiency testing by interlaboratory comparison, 2015.
[27]. AOAC INTERNATIONAL – Appendix F (Table 7) Guidelines for Standard Method Performance Requirements, 2016.

 Submit