窦银花 田怀香 郑小平

摘要 [目的]优化河虾中4种硝基呋喃的前处理方法。[方法]以标准方法中37℃的衍生温度下衍生17.0 h为对照，优化衍生温度和衍生时间，在阴性河虾中加入酸性提取液和衍生试剂2-硝基苯甲醛。[结果]在80℃的衍生温度下衍生2.0 h，提取效率和标准方法接近，反复试验6次，相对标准偏差都小于10%，除了呋喃妥因（AHD）响应偏小，相对偏差值较大。4种硝基呋喃代谢物的检出限为0.25 μg/kg，定量限为0.50 μg/kg，在标准曲线范围内线性良好，3个水平的回收率在90%～110%。[结论]该方法简单、快速、准确、可重复且灵敏，可以满足河虾中硝基呋喃残留量的监测要求。

关键词 硝基呋喃代谢物;河虾;衍生温度;衍生时间;前处理方法;优化

中图分类号 TS254.7文献标识码 A

文章编号 0517-6611（2021）02-0189-04

doi：10.3969/j.issn.0517-6611.2021.02.051

开放科学（资源服务）标识码（OSID）：

Optimization of Pretreatment Detection Methods for Four Nitrofurans in Shrimp

DOU Yinhua1，TIAN Huaixiang2，ZHENG Xiaoping1 （1.Shanghai Bino Testing Technology Service Co.，Ltd.，Shanghai 200101;2.Shanghai Institute of Technology，Shanghai 201418）

Abstract [Objective] To optimize the pretreatment methods of 4 kinds of nitrofurans in river shrimp.[Method]Taking the derivatization temperature of 37℃ in the standard method for 17.0 h as the control，the derivative temperature and time were optimized.Acid extract and derivative reagent 2nitrobenzaldehyde were added to the negative shrimp.[Result] The derivative temperature was 80℃ and the derivative time was 2.0 h， the extraction efficiency was close to the standard method，and the relative standard deviation was less than 10% after 6 times of repeated experiments，except that the response of nitrofurantoin （AHD） was smaller and the relative deviation was larger.At the same time，the experiment found that the detection limit of the four nitrofuran metabolites was 0.25 μg/kg，and the limit of quantification was 0.50 μg/kg，the linearity was good in the range of standard curve，and the recoveries of three levels were between 90% and 110%.[Conclusion]The method has the advantages of simple and fast operation，accurate results，good repeatability and high sensitivity，and can meet the monitoring requirements of nitrofuran drugs in shrimp.

Key words Nitrofuran metabolites; Shrimp; Derivative temperature; Derivative time;Pretreatment method;Optimization

硝基呋喃類药物对大多数革兰氏菌、真菌和原虫等病原体均有预防和控制的作用，是一种合成型广谱抗生素，生产成本低、药效显著、耐药性差、应用广泛，大量用于河虾和畜牧业[1-3]。硝基呋喃代谢物主要包括呋喃唑酮（AOZ）、呋喃它酮（AMOZ）、呋喃妥因（AHD）、呋喃西林（SEM），是一类带有5-硝基呋喃环结构化合物[4-5]，长期食用此类药物，会诱导有机体发生突变和癌变[6-7]。从21世纪初开始，中华人民共和国农业部公告第235号明确规定动物食品中兽药的最大残留限量，禁止在动物食品中检出硝基呋喃类兽药[8-9]。 欧盟和亚洲等许多国家也规定，硝基呋喃代谢产物在动物食品中不得检出。

截至目前，硝基呋喃代谢物的检测方法有酶联……