Validasi metode analisis kandungan spesifik residu total monomer stiren pada kemasan polistiren busa dengan simulan panga

Abstract

In the last decade, plastic food packaging safety is a part of food safety issues. One type of plastic food packaging -related safety spotlight is polystyrene packaging. Some research results showed that the styrene monomer which is the basic ingredient of polystyrene can migrate into food and cause disruption to human health such as cancer groups 2B according to International Agency for Research on Cancer (IARC), impaired estrogenic effects, genotoxic, cytotoxic and etc. Besides the health effect, the exposure to use the polystyrene packaging widespread in society, it is because of the excess of polystyrene which can maintain food hot or cold condition, maintain the freshness and integrity of packaged food, and light. Based on health effect and exposure widespread in society, the polystyrene packaging become one of the priorities of government supervision of food packaging in that case done by the National Agency of Drug and Food Control (NADFC). NADFC supervision is done through sampling and laboratory testing. In terms of supporting laboratory testing, it is necessary to increase the ability of food packaging testing in the laboratory, one of them is a set of analysis methods of food packaging testing in accordance with applicable regulatory requirements. This research aim was to conduct the analytical method validation of the determination of total residual styrene monomer in polystyrene packaging by gas chromatography - flame ionization detector (GC-FID) with heptane as a food simulant in accordance to the Decree of The Head of National Agency of Drug and Food Control Republic of Indonesia No. HK.03.1.23.07.11.6664 2011 on Food Packaging Control. The method used is divided into three (3) stages: (1) preparation stage, (2) the orientation procedure testing stage and (3) the method validation stage. The preparation stage includes the preparation of materials and checking instrument performance GC-FID. Preparation of materials is done by making the styrene standard stock solution and the internal standard stock solution of each 1000 μg/mL. While checking the performance of the GC-FID instrument used as an initial orientation to detect styrene with certain conditions and parameters that determine the linearity of the standard curve working with 5 (five) different concentrations and precision instruments and GC -FID determination of the Limit Of Detection/ LOD and Limit of Quantitation/ LOQ instrument GC-FID. Orientation procedure testing stage consists of sample preparation polystyrene packaging accordance to the Decree of The Head of National Agency of Drug and Food Control Republic of Indonesia No. HK.03.1.23.07.11.6664 2011 on Food Packaging Control and then testing the total residual styrene monomer and styrene concentration analysis in a sample of test solution by GC-FID. Method validation phase is the most crucial step in this research is to validate methods analisys of testing procedures with parameters selectivity, linearity, precision and accuracy. The results of preparation phase that used stiren standard showed that the linearity and precision met the requirements of linearity with R2 = 0.999 (requirement R2 > 0.990 ) and precision with RSD value of retention time and the area of styrene was 0.01 % and 0.61 %, whereas the internal standard 0.01 % and 0.45 %, respectively (JECFA requirements RSD values < 2.0 %). On checking the performance of the instrument determination of LOD and gave the results of LOQ is obtained LOD = 0.40 mg / mL and LOQ = 1.34 mg/ mL. In the orientation phase of the test procedure, the analysis of determination of total residual styrene monomer in foam polystyrene packaging showed the concentrations at 94.63 ± 4.73 μg/g sample. While the results of the validation of the method is having good selectivity to styrene measured quantitatively, the linearity with R2 = 0.999 (requirement R2 > 0.999), precision with the value of RSD = 0.93 % (RSD requirements < 2/3 RSD Horwitz ie 5.44 % ), accuracy percent recovery ( % recovery ) = 98.04 ± 2.62 % with spiking concentration of styrene 502 μg/g sample (AOAC requirements at a concentration of 100 μg/g = 85-110 % ), LOD = 0.15 μg/mL and LOQ = 1.20 μg/mL. Based on those results, the analytical method to determine styrene in ploystyrene packaging by GC-FID instrument is valid. The results of the validation method in this research are expected to be used as a reference for the food industry and food packaging laboratories for testing the determination of total residual styrene monomer in polystyrene packaging, this can increase the ability of laboratories in Indonesia to conduct a food packaging compliance test according to the applicable regulations.