许凯伦 蒋倩倩 郑伊诺 徐汇镔 陆荣茂 周朝生 胡园

摘要 [目的]通过固相萃取，建立超高效液相色谱-串联质谱法同时分析水体及水产品中6种喹诺酮类药物残留检测方法。[方法]水质检测方法取样量少，生物检测方法利用乙腈和水作为提取液，并添加DMSO，增进目标物在乙腈中的溶解度从而提高回收率;调查浙江省某地区20个中华鳖养殖场养殖水体和中华鳖的6种喹诺酮药物残留水平。[结果]水质检出2种喹诺酮残留，检出浓度最大值分别为421.06 ng/L（恩诺沙星）、54.20 ng/L（环丙沙星）;中华鳖样品中检出4种喹诺酮残留，最大检出浓度分别为3.98 μg/kg（氧氟沙星）、3.22 μg/kg（培氟沙星）、127.44 μg/kg（恩诺沙星）、65.00 μg/kg（环丙沙星），食品安全指数均值为0.000 7，食品安全状态较好。[结论]该方法灵敏度较高、分析时间较短、回收率较高，可以定量检测养殖水体和养殖生物体中喹诺酮类药物残留。

关键词 喹诺酮;养殖水体;中华鳖;药物残留;食品安全指数;固相萃取-超高效液相色谱-串联质谱法

中图分类号 TS254.7 文献标识码 A

文章编号 0517-6611（2021）01-0181-05

doi：10.3969/j.issn.0517-6611.2021.01.049

Abstract [Objective]A method for simultaneous detection of 6 kinds of quinolone in environmental water samples and aquatic products samples by using high performance liquid chromatography-tandem mass spectrometry was developed.[Method]The volume of water sample which was needed was small，and aquatic products samples were extracted with the mixture of acetonitrile， water and DMSO. The residue of 6 kinds of quinolone antibiotics in water in aquafarm and Trionyx sinensis in an area of Zhejiang Province was measured.[Result]2 antibiotics were detected in water samples with maximum concentrations of 421.06 ng/L（enrofloxacin），54.20 ng/L（ciprofloxacin）.4 antibiotics were detected in Trionyx sinensis with maximum concentrations of 3.98 μg/kg（ofloxacin），3.22 μg/kg （pefloxacin），127.44 μg/kg（enrofloxacin），65.00 μg/kg（ciprofloxacin）. The average number of IFS of Trionyx sinensis was 0.000 7， which was acceptable. [Conclusion]This method has high sensitivity， short analysis time and high recovery rate， and can quantitatively detect quinolone drug residues in aquaculture water and aquaculture organisms.

Key words Quinolone;Aquaculture water;Trionyx sinensis;Drug residues;IFS;Solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

抗生素能有效预防和治疗疾病，并有一定的促进生长的作用，被广泛地用于医药、畜禽水产的养殖业中。我国作为人口大国和养殖业大国，抗生素使用量巨大。2013年中国科学院广州地球化学研究所发布了全国抗生素污染地图，調查估算一年有超过5万t抗生素排放进水土环境中，其中46.1%由养殖业引起[1]，浙江属于较为严重的抗生物污染地区。

喹诺酮是一类人工合成的广谱类抗菌药，通过抑制细菌的DNA解……