Sains Malaysiana 41(11)(2012): 1451–1459


Determination of Herbicide Diuron Levels in Palm Oil Matrices using HPLC-UV

(Penentuan Aras Herbisid Diuron dalam Matriks Minyak Sawit Menggunakan HPLC-UV)


Mohd Izwarie Ramli, Tan Yew Ai & Halimah Muhamad*

Analytical and Quality Development Unit, Malaysian Palm Oil Board, No. 6, Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia


Mohd Izwarie Ramli, Zuriati Zakaria

School of Chemical Sciences and Food Technology, Faculty Science and Technology

Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia


School of Enviromental and Natural Resource Sciences

Faculty Science and Technology, Universiti Kebangsaan Malaysia

43600 Bangi, Selangor, Malaysia


Received: 19 December 2011 / Accepted: 28 June 2012



The objective of this study was to develop a method for the determination of diuron (3-(3,4-dichlorophenyl)-1,1-dimethyl urea) residue in crude palm oil (CPO) and crude palm kernel oil (CPKO) matrices. The method involves the extraction of the herbicide from the oil matrix using low temperature precipitation and solid phase extraction techniques, detected by high performance liquid chromatography-ultra violet (HPLC-UV). The HPLC separation was carried out on an AscentisTM RP-Amide column and elution with acetonitrile (solvent A) and water-methanol (2:1, v/v) (solvent B) as a suitable solvent system, at ratio of 4:6 (v/v). The optimum volume of acetonitrile for the extraction of diuron was 30 mL and 4 mL was obtained as the optimum volume of the solvent for elution analyte through the SPE cartridge. A linear correlation was obtained for the concentration of diuron from 0.05–1.0 μg mL-1 with a correlation coefficient of 0.99. The recovery of diuron from CPO was 83.2–101.4% with a relative standard deviation of 1.4–9.9% and 79.4–87.9% with relative standard deviation of 0.9–5.6% for CPKO. The method detection limit and limit of quantification obtained were 0.018 μg g-1 and 0.058 μg g-1, respectively. The method was used to determine diuron residues in palm oil from different refineries situated at different locations throughout Malaysia.


Keywords: Crude palm kernel oil; crude palm oil; diuron; herbicide



Objektif kajian ini adalah untuk membangunkan satu kaedah bagi menentukan residu diuron (3-(3,4-diklorofenil)-1,1-dimetil urea) di dalam matriks minyak sawit mentah (CPO) dan minyak isirong sawit (CPKO). Kaedah yang dibangunkan melibatkan pengekstrakan herbisid daripada matriks minyak sawit menggunakan teknik pemendakan bersuhu rendah dan pengekstrakan fasa pepejal yang dikesan dengan kromatografi tekanan prestasi tinggi-ultra lembayung (HPLC-UV). Pemisahan dengan HPLC-UV dibuat menggunakan turus AscentisTM RP-Amide dan dielusi dengan asetonitril (pelarut A) dan air-metanol (2:1, v/v) (pelarut B) sebagai sistem pelarut yang sesuai, pada nisbah 4:6 (v/v). Isi padu pelarut asetonitril optimum untuk mengekstrak diuron adalah 30 mL dan 4 mL diperoleh sebagai isi padu pelarut optimum untuk mengelut analit melalui kartrij SPE. Kolerasi lurus diperoleh pada julat kepekatan diuron 0.05–1.0 μg mL-1 dengan kolerasi koefisen 0.9983. Peratus perolehan semula diuron bagi CPO ialah 83.2–101.4% dengan sisihan piawai relatif 1.4–9.9% dan 79.4–87.9% dengan sisihan piawai relatif 0.9–5.6% bagi CPKO. Had pengesanan kaedah dan had kuantitatif yang diperoleh masing-masing adalah 0.018 μg g-1 dan 0.058 μg g-1. Kaedah yang dibangunkan digunakan untuk menentukan residu diuron di dalam minyak sawit daripada kilang penapisan yang berbeza di seluruh Malaysia.


Kata kunci: Diuron; herbisid; minyak isirong sawit; minyak sawit mentah



Ainie, K., Tan, Y.A., Norman, K. & Yeoh, C.B. 2007. Pesticide application in the oil palm plantation. Oil Palm Bull. 54: 52-67.

Aramendia, M.A., Borau, V., Lafont, F., Marinas, A., Marinas, J.M., Moreno, J.M. & Urbano, F.J. 2007. Determination of herbicide residues in olive oil by gas chromatography-tandem mass spectrometry. Food Chem. 105: 855-861.

Garcia-reyes, J.F., Ferrer, M.J., Gomez-ramos, M.J., Molina-diaz, A. & Fernandez-alba, A.R. 2007. Determination of pesticide residues in olive oil and olives. Trends in Anal. Chem. 26: 239-251.

Guardia-rubio, M., Banegas-font, V., Molina-diaz, A. & Ayora-canada, M.J. 2006a. Determination of triazine herbicides and diuron in mud from olive washing devices and soils using gas chromatography with selective detectors. Anal. Letters 39: 835-850.

Guardia-rubio, M., Fernandez-de cordova, M.L., Ayora-canada, M.J. & Ruiz-medina, A. 2006b. Simplified pesticide multiresidue analysis in virgin olive oil by gas chromatography with thermoionic spesific, electron-capture and mass spectrometric detection. J. Chromagr. A1108: 231-239.

Halimah, M., Osman, H., Ainie, K., Tan, Y.A. & Md. Pauzi, A. 1999. Determination of chlorpyrifos in refined palm olein by GC-FPD and GC-ECD. J. Palm Oil Res. 11: 89-97.

Kidd, H. & James, D.R. 1991. The Agrochemicals Handbook. 3rd Ed. Cambridge, UK: Royal Society of Chemistry.

Lentza-rizos, Ch., Avramides, E.J. & Visi, E. 2001a. Determination of residues of endosulfan and five pyrethroid insecticides in virgin olive oil using gas chromatography with electron-capture detection. J. Chromatogr. A 921: 297-304.

Lentza-rizos, Ch., Avramides, E.J. & Cherasco, F. 2001b. Low-temperature clean-up method for the determination of organophosphorus insecticides in olive oil. J. Chromatogr. A 912: 135-142.

Lin, S.W. 2011. Palm oil. In: Vegetable Oils in Food Technology: Composition, Properties and Uses. 2nd Ed. edited by Gunstone, F.D. UK: Wiley-Blackwell.

Mou, R.X., Chen, M.X. & Zhi, J.L. 2008. Simultaneous determination of 15 phenylurea herbicides detection combined with UV decomposition and post-column derivatization. J. Chromagr. B 875(2): 437-443.

MPOB. 2009. Http:// (accessed Jan 2011)

Muhamad, H., Md. Pauzi, A., Ai, T.W. & Chian, S. S. 2004. Optimization of the sweep co-distillation clean-up method for the determination of organoclorine pesticide residues in palm oil. J. Palm Oil Res. 16(2): 30-36.

Muhamad, H.B., Ai, T.Y. & Sahid, I.B. 2008. Determination of the herbicide fluroxypyr in oil matrices. J. Environ. Sci. Health B 43: 134-140.

Pihlstrom, T., Anastassiades, M., Anderson, A., Kok, A-de., Poulsen, M.E., Fernandez-alba, A.R., Gamon, M., Lippold, R., Malato, O., Medina, P., Masselter, S., Mol, H., Reynolds, S. & Valverde, A. 2009. Method validation and quality control procedures for pesticide residues analysis in food and feed. 2009. Document No. SANCO/10684/2009. protection/ resources/qualcontrol_en.pdf (accessed Sept 2010).

Shimelis, O., Yang, Y., Stenerson, K., Kaneko, T. & Ye, M. 2007. Evaluation of a solid-phase extraction dual-layer carbon/primary secondary amine for clean-up of fatty acid matrix components from food extracts in multiresidues pesticide analysis. J. Chromatogr. A1165: 18-25.

USEPA. 1994. Method detection limit, Part 136, USEPA definition in 40 CFR. Appendix B 7-1-94 Ed.

Wahab, H.A. Forages in oil palm and rubber plantations in Malaysia. 2001. (accessed June 2010).

Yeoh, C.B., Kuntom, A., Dorasamy, S., Omar, M.R., Nor, M.Y.M. & Noh, M.R.M. 2006. Determination of acephate, methamidophos and monocrotophos in crude palm oil. Eur. J. Lipid Sci. Technol. 108: 960-964.

Zainudin, B.H., Bakar, N.K.A. & Muhamad, H. 2009. Determination of cypermethrin in palm oil matrices. Eur. J. Lipid Sci. Technol. 111: 1014-1019.



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