DEVELOPMENT AND VALIDATION OF METHODS FOR ANALYSIS OF ETHYLENE GLYCOL AND DIETHYLENE GLYCOL CONTAMINATION IN FACIAL SERUM USING GC-MS

• Main Author: Restu Putriyani, Afra
• Format: Final Project
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/82680
• Institution: Institut Teknologi Bandung

In Indonesia, cosmetics, especially facial serums, are one of the products that are in demand with the various benefits they offer. When making serum, mixed solvents or additional ingredients are often used which can leave residual solvents such as ethylene glycol and diethylene glycol. Ingesting relatively high doses of diethylene glycol can cause liver and kidney damage. Meanwhile, ethylene glycol can cause mild irritation of mucous membranes or skin. The European Pharmacopoeia currently sets limits for diethylene glycol in glycerol at no more than 0.1% and in polyethylene glycol 0.4% as a total of ethylene glycol and diethylene glycol. The research aims to obtain an analytical method for determining ethylene glycol and diethylene glycol in facial serum using the GC-MS method. The research began with optimizing chromatography conditions and sample preparation, system suitability testing, and validation of analytical methods which include specificity, linearity, precision, accuracy. The sample matrix can be reduced via liquid-liquid extraction with hexane. In this study, gas chromatography was used with a DB Wax UI column of 0.25 mm x 30 m, helium carrier gas, a split ratio of 10:1, a flow rate of 0.5 mL per minute, and a mass spectrometry detector. The linearity parameter is expressed as a correlation coefficient of 0.9973 for ethylene glycol and 0.9953 for diethylene glycol. The detection limit and quantitation limit for ethylene glycol are 1.299 µg/mL and 3.170 µg/mL respectively, while for diethylene glycol it is 3.435 µg/mL and 7.936 µg/mL. In the repeatability precision test, the %RSD values for ethylene glycol and diethylene glycol were 5.535% and 6.508% respectively, while the intermediate precision %RSD values for ethylene glycol and diethylene glycol were 6.524% and 3.901% respectively. Accuracy test results are expressed as % recovery of ethylene glycol and diethylene glycol, respectively in the range of 90.7 – 100.4% and 95.1 – 111.2%. Based on the overall results, it can be concluded that the analytical method has been successfully developed and validated and can be used to determine ethylene glycol and diethylene glycol in facial serum. The levels of ethylene glycol and diethylene glycol in the facial serum products tested were in the range of 0.001% - 0.258%.