ARTICLE IN PRESS

DEVELOPMENT AND VALIDATION OF AN LCMS/ MS METHOD FOR DETERMINATION OF RESIDUAL 2,4-DICHLOROPHENOXYACETIC ACID HERBICIDE IN PALM OIL

NAJWA SULAIMAN1*; YEOH CHEE BENG1; NIK SASHA KHATRINA KHAIRUDDIN1 and FARAH KHUWAILAH AHMAD BUSTAMAM1

DOI: https://doi.org/10.21894/jopr.2021.0042
Published Online: 26 October 2021
ABSTRACT

2,4-dichlorophenoxyacetic acid (2,4-D) is listed as one of the most widely used herbicides in Malaysian oil palm plantation and hence it is important to use validated methods for analysis of possible pesticide contamination in palm oil supply chain. This article reports on the development of an analytical method for the determination of residual 2,4-D in crude palm oil (CPO) using a liquid chromatography tandem mass spectrometry quadrupole time of flight (LC-QToF-MS). The method of analysis was based on a liquid-liquid extraction using methanol, heating of samples and low temperature precipitation technique. Evaluation of validation parameters such as linearity, matrix effect, selectivity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery for CPO were performed. The results showed good linearity with average coefficient of determination (r2) of more than 0.99. The LOD and LOQ for analysis of residual 2,4-D was estimated at 5.0 and 10.0 ng g–1, respectively. Acceptable recoveries between 85% and 117%, repeatability with good relative standard deviation (RSD) of 5% to 10% and intermediate precision with RSD of less than 11% were obtained. Random monitoring of CPO showed that 2,4-D was not detected in any of the CPO samples.

KEYWORDS:


1 Malaysian Palm Oil Board, 6 Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia.

* Corresponding author e-mail: najwa.sulaiman@mpob.gov.my