Validation of The Modified Weihaar’s Method for the Determination of 3-Monochloropropane-1,2-Diol (3-MCPD) and Its Ester in Palm oil.

Abstract

Food safety problems may occur throughout the food chain from farm to fork. Food Law (law No. 18, 2012) stated that food safety is condition and efforts needed to prevent food from contamination of biological, chemical and other agents, that may interfere, harm, and harmful to human health and do not contradict with religions, beliefs, and culture of the society so that it will be safe to be consumed. The compound of 3-monochloropropane-1,2-diol (3-MCPD) and its ester are contaminants formed during the food processing. Both of these compounds are found in vegetables oil and some processed food, especially food processed using heat in the production process. The mechanism of 3-MCPD formation and its esters has not been fully established. It has been hypothesized that 3-MCPD was formed by reaction between chlorine and lipids during cooking and storage process of food, that may be trigered by heat or enzyme-catalyzed reaction. Consequently, validated analytical method for analysis of 3-MCPD and its ester is needed. The research aims were to validate the modified Weihaar's method of analysis of 3-MCPD and 3-MCPD esters in refined palm oil. The research was conducted in three main stages including determining the analysis method to determine the levels of 3-MCPD and its esters in palm oil using GC-MS; validation of analysis methods; and determining the levels of 3-MCPD in several product of palm oil. Validation result shows the following: A linear regression line has an equation of the form y = 0.076x + 0.005, where x is area ratio of standard external and standard internal and y is concentration ratio of external standard and internal standard. The linearity was showed by corelation coefficient (r) 0.994; linear response was obtained between 0.008 and 0.377 mg/L; limit of detection was 0.06 mg/kg, limit of quantification was 0.20 mg/kg, precision (relative standard deviation (RSD)) was 6.16%, and accuracy (as percentage of recovery) was in range 95.83-113.27%. This result indicated that the modified method was valuable and sensitive for detection of 3-MCPD and 3-MCPD esters. Using the validated method, the 3-MCPD esters in commercial palm oil sample determined and calculated as the difference between total 3-MCPD and free 3-MCPD, was 13.24 mg/kg. The total 3-MCPD in several palm oil give result on concentration range 13.94-34.52 mg/kg. These results also showed that there was a correlation between 3-MCPD with diacylglyceride (DAG). The sampel with high DAG contents give a high test results of 3-MCPD, this relationship was expressed by the coefficient of correlation (r) 0.752.