Development of LC-MS/MS Quantitation Method for Ethoxyquin in Fishery Products
2016
Shin, D., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Chae, Y.S., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Kang, H.S., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Lee, S.B., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Cho, Y.J., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Cheon, S.Y., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Jeong, J., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Rhee, G.S., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea
Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient (r²) greater than 0.99, analyzed at 0.005- 0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.
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