超高效液相色谱-串联质谱法测定淡水鱼中硝基呋喃类代谢物残留

Determination of nitrofuran metabolites residues in freshwater fishes by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  硝基呋喃类代谢物  淡水鱼  兽药残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  nitrofuran metabolites  freshwater fishes  veterinary drugs residue

中文摘要:

      目的 建立超高效液相色谱-串联质谱测法测定淡水鱼中呋喃它酮、呋喃妥因、呋喃唑酮和呋喃西林等硝基呋喃代谢物的研究方法。方法 样品中加入同位素内标, 经盐酸水解, 用2-硝基苯甲醛衍生, 乙酸乙酯液-液萃取净化后, 超高效液相色谱-串联质谱仪测定, 内标法定量。结果 4种硝基呋喃代谢物的检出限为0.07~0.25 μg/kg; 在0.1~10 ng/mL范围内线性相关系数r>0.996; 4种硝基呋喃代谢衍生物的加标回收率分别为94.0%~98.2%、84.0%~89.6%、94.0%~99.0%和75.4%~85.5%; 相对标准偏差为2.5%~9.2%。应用建立的方法对48份淡水鱼进行测定, 其中1份检出呋喃唑酮代谢物3-氨基-2-噁唑烷基酮(3-amino-2-oxazolidinone, AOZ), 含量为0.45 μg/kg。结论 建立的方法选择性高、灵敏性强、准确度高, 能满足淡水鱼中硝基呋喃类代谢物残留的高灵敏分析。

英文摘要:

      Objective To establish a method for determination of nitrofuran metabolites of nitrofurantoin (AMOZ) , nitrofurazone (AHD), furazolidone (AOZ) and furaltadone (SEM)in freshwater fishes by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples with isotope internal standard solutions were hydrolyzed by hydrochloric acid and were derivatized by 2-nitrobenzaldehyde. The analysts were cleaned up by liquid-liquid extraction with ethyl acetate, determined by ultra performance liquid chromatography-tandem mass spectrometry and simultaneously quantified by the isotope internal standard. Results The limits of detection of 4 nitrofuran metabolites ranged from 0.07 to 0.25 μg/kg. The standard curves were linear in the range of 0.1~10 ng/mL, and the correlation coefficients r>0.996. The average recoveries for 4 kinds of nitrofuran metabolites were 94.0%~98.2%, 84.0%~89.6%, 94.0%~99.0% and 75.4%~85.5%, respectively. The relative standard deviations varied between 2.5% and 9.2%. The method was applied to analyze 48 fish samples, and one of which was confirmed to contain AOZ of 0.45 μg/kg. Conclusion The method is selective, sensitive and accurate, which is suitable for trace analysis of nitrofuran metabolites in freshwater fishes.