Halimah Muhamad

Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry

An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl.

Determination of the herbicide fluroxypyr in oil matrices

The purpose of this study was to develop a method for the determination of fluroxypyr (4-amino-3,5-dichloro-6-fluro2-pyridyloxyacetic acid) residue in palm oil namely crude palm oil (CPO) and crude palm kernel oil (CPKO). The method involves the extraction of the herbicide from the oil matrix followed by low temperature precipitation and finally quantification of the residues using the high performance liquid chromatography (HPLC). The extraction efficiency of the method was evaluated by conducting recovery studies. The recovery of fluroxypyr from the fortified CPO samples ranged from 78%–111% with the relative values for the coefficient of variation ranging from 1.4 to 8.6%. Furthermore, the recovery of fluroxypyr from the spiked CPKO samples ranged from 91–107% with the relative values for the coefficient of variation ranging from 0.6 to 4.5%. The minimum detection limit of fluroxypyr in CPO and CPKO was 0.05 μg/g. The method was used to determine fluroxypyr residues from the field-treated samples of CPO and CPKO. When fluroxypyr was used for weed control in oil palm plantations no residue was detected in CPO and CPKO irrespective of the sampling interval and the dosage applied at the recommended or double the manufacturers recommended dosage.

Effects of temperature and NaCl on the formation of 3-MCPD esters and glycidyl esters in refined, bleached and deodorized palm olein during deep-fat frying of potato chips

The effects of frying duration, frying temperature and concentration of sodium chloride on the formation of 3-monochloropropane-1,2-diol (3-MCPD) esters and glycidyl esters (GEs) of refined, bleached and deodorized (RBD) palm olein during deep-fat frying (at 160°C and 180°C) of potato chips (0%, 1%, 3% and 5% NaCl) for 100min/d for five consecutive days in eight systems were compared in this study. All oil samples collected after each frying cycle were analyzed for 3-MCPD esters, GEs, free fatty acid (FFA) contents, specific extinction at 232 and 268 nm (K232 and K268), p-anisidine value (pAV), and fatty acid composition. The 3-MCPD ester trend was decreasing when the frying duration increased, whereas the trend was increasing when frying temperature and concentration of NaCl increased. The GEs trend was increasing when the frying temperature, frying duration and concentration of NaCl increased. All of the oil qualities were within the safety limit.

Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia.

Determination of hexaconazole in field samples of an oil palm plantation

In oil palm plantations, the fungicide hexaconazole is used to control Ganoderma infection that threatens to destroy or compromisethe palm. The application of hexaconazole is usually through soil drenching, trunk injection, or a combination of these two methods. It is therefore important to have a method to determine the residual amount of hexaconazole in the field such as in samples of water, soil, and leaf to monitor the use and fate of the fungicide in oil palm plantations. This study on the behaviour of hexaconazole in oil palm agro-environment was carried out at the UKM-MPOB Research Station, Bangi Lama, Selangor. Three experimental plots in this estate with 7-year-old Dura x Pisifera (DxP) palms were selected for the field trial. One plot was sprayed with hexaconazole at the manufacturers recommended dosage, one at double the recommended dosage, and the third plot was untreated control. Hexaconazole residues in the soil, leaf, and water were determined before and after fungicide treatment. Soil samples were randomly collected from three locations at different depths (0-50 cm) and soil collected fromthe same depth were bulked together. Soil, water, and palm leaf were collected at -1 (day before treatment), 0 (day of treatment), 1, 3, 7, 14, 21, 70, 90, and 120 days after treatment. Hexaconazole was detected in soil and oil palm leaf, but was not detected in water from the nearby stream.

New Insights on Degumming and Bleaching Process Parameters on The Formation of 3-Monochloropropane-1,2-Diol Esters and Glycidyl Esters in Refined, Bleached, Deodorized Palm Oil

This paper examines the interactions of degumming and bleaching processes as well as their influences on the formation of 3-monochloropropane-1,2-diol esters (3-MCPDE) and glycidyl esters in refined, bleached and deodorized palm oil by using D-optimal design. Water degumming effectively reduced the 3-MCPDE content up to 50%. Acid activated bleaching earth had a greater effect on 3-MCPDE reduction compared to natural bleaching earth and acid activated bleaching earth with neutral pH, indicating that performance and adsorption capacities of bleaching earth are the predominant factors in the removal of esters, rather than its acidity profile. The combination of high dosage phosphoric acid during degumming with the use of acid activated bleaching earth eliminated almost all glycidyl esters during refining. Besides, the effects of crude palm oil quality was assessed and it was found that the quality of crude palm oil determines the level of formation of 3-MCPDE and glycidyl esters in palm oil during the high temperature deodorization step of physical refining process. Poor quality crude palm oil has strong impact towards 3-MCPDE and glycidyl esters formation due to the intrinsic components present within. The findings are useful to palm oil refining industry in choosing raw materials as an input during the refining process.

Life cycle inventory of oil palm lumber production: A gate-to-gate case study

Life Cycle Assessment (LCA) has been applied in the Malaysian oil palm industry since 2010. It is important to ensure that this main industry is ready to meet the demands and expectations of European market on the environmental performance of the oil palm industry. In addition, oil palm biomass, especially oil palm trunk (OPT) are abundantly available after replanting every year. In order to maximize the usage of OPT as a green product, it can be converted to palm lumber as a value-added product. Palm lumber act as a basis product from OPT before it is converted to panel product such as plywood, sandwich board and so on. However, the LCA study on palm lumber production is still scarce in Malaysia. Hence, this paper aims to perform and collect the inventory data for palm lumber production, which is known as Life Cycle Inventory (LCI). A gate-to-gate system boundary and the functional unit of 1 m3 of palm lumber produced have been used in this study. This inventory data was collected from three batches of the production cycle. The inputs are mainly the raw materials which are the OPT and the energy from diesel and electricity from the grid. Generally, each consumption of input such as energy and fossil fuel were different at each stage of palm lumber production. Kiln-drying represents a prominent stage in terms of energy consumption, which electrical use in the dryer represents 94% of total electrical grid consumption as compared to another stage of palm lumber production. By adding the inventory information especially in the downstream sector of biomass industry, hopefully it can improve the sustainability of oil palm industry in Malaysia.Life Cycle Assessment (LCA) has been applied in the Malaysian oil palm industry since 2010. It is important to ensure that this main industry is ready to meet the demands and expectations of European market on the environmental performance of the oil palm industry. In addition, oil palm biomass, especially oil palm trunk (OPT) are abundantly available after replanting every year. In order to maximize the usage of OPT as a green product, it can be converted to palm lumber as a value-added product. Palm lumber act as a basis product from OPT before it is converted to panel product such as plywood, sandwich board and so on. However, the LCA study on palm lumber production is still scarce in Malaysia. Hence, this paper aims to perform and collect the inventory data for palm lumber production, which is known as Life Cycle Inventory (LCI). A gate-to-gate system boundary and the functional unit of 1 m3 of palm lumber produced have been used in this study. This inventory data was collected from three batches of t...

Life cycle inventory for palm based plywood: A gate-to-gate case study

The oil palm industry heavily relies on the world market. It is essential to ensure that the oil palm industry is ready to meet the demands and expectation of these overseas customers on the environmental performance of the oil palm industry. Malaysia produces 13.9 million tons of oil palm biomass including oil palm trunk (OPT), frond and empty fruits bunches (EFB) annually. OPT felled in some oil palm plantations during replanting is transported to various industries and one such industry is the plywood factories. In order to gauge the environmental performance of the use of OPT as plywood a Life Cycle Assessment (LCA) study was conducted for palm based plywood. LCA is an important tool to assess the environmental performance of a product or process. Life cycle inventory (LCI) is the heart of a LCA study. This LCI study has a gate-to-gate system boundary and the functional unit is 1 m3 palm plywood produced and covers three types of plywood; Moisture Resistance Plywood (MR), Weather Boiling Proof Plywood...

Life cycle inventory for the production of germinated oil palm seeds at a selected seed production unit in Malaysia

The increasing global demand for edible oil has encouraged Malaysia to increase the areas under oil palm cultivation. The total demand for germinated oil palm seeds in the years 2009, 2010, 2011 and 2012 were 86.4, 76.5, 72.6 and 75.2 million, respectively. Production of germinated oil palm seeds is the first link in the palm oil supply chain. Therefore, good management practices at seed production stage is required to ensure only high quality germinated oil palm seeds are produced before sale to customers. Life cycle assessment (LCA) has been used as a tool to assess environmental impact of the processes throughout a products lifespan and this approach is an important tool for assessing green house gas (GHG) emission. For this study, a gate-to-gate life cycle inventory (LCI) of a single germinated oil palm seed production unit was carried out. The functional unit used for this LCI was one germinated oil palm seed. To determine the environmental impact for the production of germinated oil palm seeds, information on the inputs were obtained. The inputs for the production of germinated oil palm seeds involved materials such as polyethylene bags, electricity, water, chemicals and fungicides. For this study, the system boundary involved seed germination process and management of germinated oil palm seeds. It was found that the amount of input such as materials and energy used in the production of germinated oil palm seeds was very minimal.