Study On Detection Methods Of Nitrofuran Antibiotics In Marine Culture Sediments

Nitrofuran antibiotics are broad-spectrum antibiotics with low price and high antibacterial efficiency,for which they have been widely used in mariculture.Due to their carcinogenicity and mutagenicity to human body,The EU has completely banned nitrofuran antibiotics in 1997.However,marine organism metabolize such antibiotics quickly and it is difficult to detect the original residue in the marine foods.After these antibiotics entering the water body,those drugs that are not absorbed by organisms will be deposited in the cultured sediment.Therefore,detecting the residual drug residues of the nitrofuran antibiotics in the sediment is an important means to ensure the safety of marine foods.In this paper,the cultured sediment of Dalian sea cucumber was analyzed,and a set of detecting methods for the residues of nitrofuran antibiotics in the sediment was established.The main research results are as follows:(1)This study established a method for rapid extraction and purification of furazolidone,nitrofurantoin,and nitrofurazone in sediment.The sediment sample was extracted and purified by HLB solid phase extraction column.Simultaneous detection and quantitative analysis of three antibiotics are conducted by HPLC.These three antibiotics can be effectively separated under the mobile phase of acetonitrile/water(4/6).The experiment also investigated the recovery rates at different levels of addition,the recovery rate of furazolidone was 81% ± 0.103,nitrofurantoin was 78% ± 0.0876,nitrofurazone was 83% ± 0.118,relative standard deviation of three samples are less than 10% at the lowest addition level of 1 ng/g.Results showed that the method with high recovery and good stability.The method proposed in this study had high accuracy and good precision,which was suitable for rapid detection of nitrofuran antibiotics in the sediment simultaneously.(2)The surface-enhanced Raman(SERS)detection method for nitrofuran antibiotics was studied.The SERS signals of various nanoparticles against furan antibiotics were screened,and the gold nanoparticles were well-adjusted to the target antibiotics.The gold nanoparticles were optimized and the optimal detection conditions were explored.The gold nanoparticles were used as the SERS substrate,the mixing ratio of the target sample to the substrate was 2:1,the detection limit of furazolidone was 0.1 ?g/mL,and the detection limits of nitrofurantoin and nitrofurazone were 1 ?g/mL.This study established a set of detecting methods for the nitrofuran antibiotic residues in cucumber cultural sediment,which enable random sampling and monitoring the usage of such antibiotics in marine culture.