Optimasi dan Validasi Metode KCKT untuk Identifikasi dan Penetapan Kadar Metabolit Nitrofuran dalam Bakso Udang

Abstract

Abstract Background: Furazolidone, furaltadone, and nitrofurantoin are nitrofuran antibiotics still illegally used as food additives in shrimp farming and other food-producing animals. Therefore, due to their carcinogenicity, it is needed to control the contamination of nitrofuran metabolites in food products containing shrimps as the main ingredient. Objective: This study aimed to validate the HPLC method for determining levels of nitrofuran metabolites in shrimp meatballs. Methods: Furazolidone, furaltadone and nitrofurantoin were derivatized with 2- nitrobenzaldehyde, extracted into ethyl acetate, washed with hexane, and applied to HPLC with UV-PDA detector. The separation was performed on C-18 column 46 x 250 mm, 5 μm using the mobile phase of 20 mM ammonium acetate and acetonitrile (70:30), with a 0.5 mL/min flow rate column temperature of 40oC, injection volume of 100 μL. Results: The method showed good separation of metabolites and other interferences with an analysis time of 40 minutes, resulting in good linear response in the concentration ranges of 51.90 – 103.79 ng/mL (AOZ); 56.63 - 101.39 ng/mL (AMOZ); dan 49.92 – 89.86 ng/mL (AHD). The accuracy was found to be 78.50 - 102.29% for AOZ; 77.02 - 99.87% for AMOZ; and 85.54 - 99.77% for AHD; whereas the precision (RSD) for the repeatability test was 6.10 - 19.90%; 3.68 - 17.75%; and 2.75 - 12.58% for AOZ, AMOZ and AHD. LOD and LOQ obtained were between 3.09 and 10.29 ng/mL (AOZ); 6.84 and 22.82 ng/mL (AMOZ); and 4.61 and 15.36 ng/mL (AHD). Conclusion: The proposed method can detect and quantify nitrofuran metabolite contamination in shrimp meatballs. Keywords: AHD, AMOZ, AOZ, high-performance liquid chromatography, nitrofuran