Quantification of Some Pesticide Residues in Milk Powder in Iraq by Gas Chromatography/ Mass Spectrometry


Published: 2023-09-18

DOI: 10.56557/upjoz/2023/v44i203654

Page: 130-137

Ali Abdulla Ali *

Department of Food Science and Quality Control, College of Agricultural Engineering Science, University of Sulaimani, Sulaymaniyah, Iraq.

Khulod Ibrahim Hassan

Department of Food Science and Quality Control, College of Agricultural Engineering Science, University of Sulaimani, Sulaymaniyah, Iraq.

*Author to whom correspondence should be addressed.


Pesticides are widely used on a global scale to improve productivity, but the persistent chemical residues they leave behind contaminate the environment and pose health risks to people. As a result, the current investigation was carried out to QuEChERS procedure adapted to gas chromatography coupled with mass spectrometry (GC–MS), to monitor the amounts of several organochlorine pesticides (OC), organophosphorus pesticides (OP), and pyrethroid in milk brand powder samples that were collected from Sulaimani market. About ten milk brand samples were analyzed to detect and quantify BHC, Chlorpyrifos, α-Cypermethrin, 2,4-D, Diazinon, and Endosulfan sulphate. Analytes provided acceptable responses at validation levels of 0.05 to 1 mg/kg. The linearity correlation coefficient R² was ≥ 0.9441, and limits of detection (LOD) value ranged from 0.18-0.49, limit of quantification (LOQ) value ranged from 0.54-1.49. Recovery percentage was obtained for all spiked levels (72.57-119.3) with acceptable relative standard deviation (RSD). The compounds α-Cypermethrin and Endosulfan sulphate found in most of the milk brands after that 2,4-D was found in brands but no one of them exceeded the MRL in all milk brands.

Keywords: Dairy science, milk products, pesticide, milk powder, GC–MS, spectrometry, gas chromatography

How to Cite

Ali , A. A., & Hassan , K. I. (2023). Quantification of Some Pesticide Residues in Milk Powder in Iraq by Gas Chromatography/ Mass Spectrometry. UTTAR PRADESH JOURNAL OF ZOOLOGY, 44(20), 130–137. https://doi.org/10.56557/upjoz/2023/v44i203654


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El-Khair A, Abdalla AK, Radwan FME, Abd-El-Allah AA. Evaluation of some chemical properties of milk powders currently available at local market in Egypt. Egyptian Journal of Dairy Science. 2021;2.

Britt JH, Cushman RA, Dechow CD, Dobson H, Humblot P, Hutjens MF, Jones GA, Ruegg PS, Sheldon IM, Stevenson JS. Invited review: Learning from the future—A vision for dairy farms and cows in 2067. Journal of dairy science. 2018;101(5):3722-3741.

Deguine JP, Aubertot JN, Flor RJ, Lescourret F, Wyckhuys KA, Ratnadass A. Integrated pest management: Good intentions, hard realities. A review. Agronomy for Sustainable Development. 2021;41(3):38.

Akhtar S, Ahad K. Pesticides residue in milk and milk products: Mini review. Pakistan Journal of Analytical & Environmental Chemistry. 2017;18(1):37-45.

Rani L, Thapa K, Kanojia N, Sharma N, Singh S, Grewal AS, Srivastav AL, Kaushal J. An extensive review on the consequences of chemical pesticides on human health and environment. Journal of cleaner production. 2021;283: 124657.

Thompson LA, Darwish WS. Environmental chemical contaminants in food: review of a global problem. Journal of Toxicology. 2019;1-14.

Samsidar A, Siddiquee S, Shaarani SM. A review of extraction, analytical and advanced methods for determination of pesticides in environment and foodstuffs. Trends in Food Science & Technology. 2018;71:188-201.

Pico Y, Alfarhan AH, Barcelo D. How recent innovations in gas chromatography-mass spectrometry have improved pesticide residue determination: An alternative technique to be in your radar. TrAC Trends in Analytical Chemistry. 2020;122:115720.

Hamadamin AY, Hassan KI. Gas chromatography–mass spectrometry based sensitive analytical approach to detect and quantify non-polar pesticides accumulated in the fat tissues of domestic animals. Saudi Journal of Biological Sciences. 2020;27(3):887- 893.

Pourasil RSM, Cristale J, Lacorte S, Tauler R. Non-targeted Gas Chromatography Orbitrap Mass Spectrometry qualitative and quantitative analysis of semi-volatile organic compounds in indoor dust using the Regions of Interest Multivariate Curve Resolution chemometrics procedure. Journal of Chromatography A. 2022; 1668:462907.

Wu Z, Peng X, Chen S, Zeng Z. Determination of 19 organochlorine pesticides residues in milk powder by GPC-GC-MS. International Journal of Nutrition and Food Sciences. 2018;7(4):129-133.

González-Curbelo MÁ, Socas-Rodríguez B, Herrera-Herrera AV, González-Sálamo J, Hernández-Borges J, Rodríguez-Delgado MÁ. Evolution and applications of the QuEChERS method. TrAC Trends in Analytical Chemistry. 2015;71:169-185.

Rejczak T, Tuzimski T. QuEChERS-based extraction with dispersive solid phase extraction clean-up using PSA and ZrO2-based sorbents for determination of pesticides in bovine milk samples by HPLC-DAD. Food chemistry. 2017;217:225-233.

Tankiewicz M, Berg A. Improvement of the QuEChERS method coupled with GC–MS/MS for the determination of pesticide residues in fresh fruit and vegetables. Microchemical Journal. 2022;181:107794.

Wang W, Xiong P, Zhang H, Zhu Q, Liao C, Jiang G. Analysis, occurrence, toxicity and environmental health risks of synthetic phenolic antioxidants: A review. Environmental Research. 2021;201:111531.

Tripathy V, Sharma KK, Yadav R, Devi S, Tayade A, Sharma K, Pandey P, Singh G, Patel AN, Gautam R. et al. Development, validation of quechers-based method for simultaneous determination of multiclass pesticide residue in milk, and evaluation of the matrix effect. J. Environ. Sci. Health Part B. 2019;54:394–406.

Zheng W, Choi J, Abd El-Aty AM, Yoo K, Park D, Kim S, Kang YHacımüftüoğlu A, Wang J, Shim J. et al. Simultaneous determination of spinosad, temephos, and piperonyl butoxide in animal-derived foods using LC–MS/MS. Biomed. Chromatogr. 2019;33:e4493.

Jadhav MR, Pudale A, Raut P, Utture S, Shabeer TA, Banerjee K. A unified approach for high-throughput quantitative analysis of the residues of multi-class veterinary drugs and pesticides in bovine milk using LC-MS/MS and GC–MS/MS. Food Chemistry. 2019;272:292-305.

Shamsipur M, Yazdanfar N, Ghambarian M. Combination of solid-phase extraction with dispersive liquid–liquid microextraction followed by GC–MS for determination of pesticide residues from water, milk, honey and fruit juice. Food chemistry. 2016;204:289-297.

Shariati S, Hashemi M, Rashedinia M, Mahdavinia M, Noori SMA. Determination of 323 Pesticide Residues in Iran's Cereal by GC-MS and HPLC-UV Combined with QuEChERS Extraction and Mixed-Mode SPE Clean-Up Method; 2023.

Oymen B, Aşır S, Türkmen D, Denizli A. Determination of multi-pesticide residues in honey with a modified QuEChERS procedure followed by LC-MS/MS and GC-MS/MS. Journal of Apicultural Research. 2022;61(4): 530-542.

Lehotay SJ, Anastassiades M, Majors RE. The QuEChERS Revolution, Chromatography Online; 2010 September 1.

Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J. AOAC Int. 2003;86(2):412-31.

PMID: 12723926.

Musarurwa H, Chimuka L, Pakade VE, Tavengwa NT. Recent developments and applications of QuEChERS based techniques on food samples during pesticide analysis. Journal of Food Composition and Analysis. 2019;84: 103314.

Marson BM, Concentino V, Junkert AM, Fachi MM, Vilhena RO, Pontarolo R. Validation of analytical methods in a pharmaceutical quality system: An overview focused on HPLC methods. Química Nova. 2020;43:1190-1203.

Zheng G, Han C, Liu Y, Wang J, Zhu M, Wang C, Shen Y. Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry. Journal of dairy science. 2014;97(10):6016-6026.

Singh S, Panchal RR, Joshi MN, Litoriya NS, Shah PG. Development and validation of a fast multiresidue method for organochlorine pesticides from high fat milk with QuEChERS approach. Pesticide Research Journal. 2012;24(2):205-211.

Manav ÖG, Dinç-Zor Ş, Alpdoğan G. Optimization of a modified QuEChERS method by means of experimental design for multiresidue determination of pesticides in milk and dairy products by GC–MS. Microchemical Journal. 2019;144:124- 129.

Ibrahim SM, Salih EA, Sharif TK, Ahmed AI, Jessim AI. Investigation of some pesticide residues in full cream milk from Baghdad's markets. International Journal for Sciences and Technology. 2015; 143(2013):1-14.

Jin G, Zhang W. Determination of 19 Organochlorine Pesticide Residues in Sargassum Fusiforme by GC-MS. China Pharmacist, 2017;2173-2176.

Dobrinas S, Soceanu A, Popescu V, Coatu V. Polycyclic aromatic hydrocarbons and pesticides in milk powder. Journal of Dairy Research. 2016;83(2):261-265.

Cheema HK, Kang BK, Singh B. Residues of chlorpyriphos in bovine milk in Punjab, India. Pesticide Research Journal. 2005;17(2):87-89.

Dos Santos JS, Schwanz TG, Coelho AN, Heck-Marques MC, Mexia MM, Emanuelli T, Costabeber I. Estimated daily intake of organochlorine pesticides from dairy products in Brazil. Food Control. 2015;53:23-28.

Zhou P, Wu Y, Yin S, Li J, Zhao Y, Zhang L, Chen H, Liu Y, Yang X, Li X. National survey of the levels of persistent organochlorine pesticides in the breast milk of mothers in China. Environmental Pollution. 2011;159(2): 524-531.

Codex alimentary.

Available: https://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/en/.

EC (Commission Regulation) No 149/2008 of 29 January 2008 amending Regulation (EC) No 396/2005 of the European Parliament and of the Council by establishing Annexes II, III, and IV setting maximum residue levels for products covered by Annex I (Official Journal L58/1,1.3.2008).

European Comission. Commission Implementing Regulation (EU) 2019/533 of 28 March 2019 Concerning a Coordinated Multiannual Control Programme of the Union for 2020, 2021 and 2022 to Ensure Compliance with Maximum Residue Levels of Pesticides and to Assess the Consumer Exposure; European Commission: Brussels, Belgium, 2019. [Google Scholar]