鲜冻水产品中违禁兽药残留高效液相色谱-串联质谱法比较与改进研究

Compared and Improved Research for Determination of Contraband Veterinary Drug Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

本文对硝基呋喃类代谢物、孔雀石绿及其代谢物、氯霉素等兽药残留的检测方法进行改进,并与现行的标准方法进行比较,结果显示,优化后的检测方法,各组分的线性良好,相关系数均在0.999以上,回收率高,检出限比标准方法低,其中硝基呋喃类代谢物(AOZ、AMOZ、SEM、AHD)的检出限分别为0.15μg/kg,0.10μg/kg,0.15μg/kg,0.15μg/kg,孔雀石绿及其代谢物(MG、LMG)的检出限均为0.15μg/kg;氯霉素的检出限达到0.05μg/kg,测定结果准确可靠,结果偏差符合方法学要求。经测定,在100批次水产品中,17批次检出了兽药残留,不合格率17.0%,其中淡水鱼类为12批次,淡水鱼不合格率25.5%,海水鱼5批次,海水鱼不合格率15.2%。主要检出的是硝基呋喃类代谢物和隐色孔雀石绿,情况严重,亟待解决。建议加强多宝鱼、桂鱼、鲈鱼、柴鱼、黄鸭叫的进货把关,杜绝兽药残留不合格的水产品流入湖南市场,同时监管部门加强对超市、农产品批发市场及农贸市场水产品的监管力度,确保湖南水产品的安全。

Methods of determination of veterinary drug residue such as nitrofuran metabolites, malachite green as well as its metabolites and chloromycetin were used after comparison and optimization. Results show that components of linearity are good, correlation coefficients were higher than 0.999. the recovery rate were high, detection limit were lower than the standard method, the detection limits was 0.15 μg/kg,0.10 μg/kg,0.15 μg/kg,0.15 μg/kg of the nitrofuran metabolites(AOZ、AMOZ、SEM、AHD), 1.2 μg/kg、1.4 μg/kg of malachite green and its metabolites(Mg and LMG); chloramphenicol detection limit reached 0.05 μg/kg, test results are accurate and reliable, the result of the deviation in line with the requirements of methodology.As a result, veterinary drug residue has been tested positive for 17 batches with unsatisfactory rate 17.0% among which freshwater fish accounts for 12 batches with unsatisfactory rate 25.5% compared with marine fish accounting for 5 batches, unsatisfactory rate 15.2%. Nitrofuran metabolites and leuco-malachite green failing to meet the standard are the main causes responsible for the unsatisfactory rate which is in urgent situation and demanding prompt solvent. Stricter evaluation is supposed to be taken during the purchase of turbot 、 mandarin fish, perch 、katsuobushi 、 yellow cartfish in order to prohibit the entrance of unqualified aquatic product in Hunan market. Supervision has to be strengthened in supermarket, wholesale market and farmers market, ensuring the safety of aquatic product in Hunan market.