Development and validation of an LC-MS/MS method for determination of residual 2 4-dichlorophenoxyacetic acid herbicide in palm oil

Najwa Sulaiman, . and Yeoh Chee Beng, . and Nik Sasha Khatrina Khairuddin, . and Farah Khuwailah Ahmad Bustamam, . Development and validation of an LC-MS/MS method for determination of residual 2 4-dichlorophenoxyacetic acid herbicide in palm oil. pp. 348-355. ISSN 2811-4701

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 (r) 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“ 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.

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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 (r) 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“ 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.

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Item Type:	Article
AGROVOC Term:	Palm oils
AGROVOC Term:	Plantations
AGROVOC Term:	2 4-dichlorophenoxyacetic acid
AGROVOC Term:	Herbicides
AGROVOC Term:	detect
AGROVOC Term:	Evaluation
AGROVOC Term:	Contaminants
AGROVOC Term:	Contamination
Depositing User:	Mr. AFANDI ABDUL MALEK
Last Modified:	24 Apr 2025 00:55
URI:	http://webagris.upm.edu.my/id/eprint/10683

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