超高效液相色谱-_串联质谱法测定鱼肉中4_种四环素类抗生素

超高效液相色谱-_串联质谱法测定鱼肉中4_种四环素类抗生素

养殖与饲料2023年第5期

收稿日期：2022-10-11作者简介：王雪蓉，女，1995年生，助理工程师。*通信作者：马义虔，男，1989年生，硕士，中级工程师。

超高效液相色谱-串联质谱法测定

鱼肉中4种四环素类抗生素

王雪蓉，杨燕红，杨丽，陈大鹏，马义虔*

贵州省产品质量检验检测院，贵阳550016

摘要[目的]建立超高效液相色谱-串联质谱同时测定鱼肉中4种四环素类抗生素（四环素、金霉素、土霉

素、强力霉素）的方法。[方法]样品经Na 2EDTA-Mcllvaine 缓冲溶液提取，正己烷除油脂，经Oasis HLB 固相萃取小柱净化，采用ACQUITY UPLC R BEH C18色谱柱(2.1mm ×50mm ，1.7μm )分离。[结果]四环素、金霉素、土霉

素、强力霉素4种四环素类抗生素在0~100ng/mL 范围内线性关系良好，相关系数（）均大于0.999；在5.0~50.0μg/kg 添加水平下，回收率均在70%~120%；相对偏差（RSD ）均小于10%；检出限为5.0μg/kg ，定量限为10.0μg/kg 。[结论]超高效液相色谱-串联质谱法可用于鱼肉中四环素类抗生素的测定。

关键词超高效液相色谱-串联质谱法；鱼肉；四环素；金霉素；土霉素；强力霉

素

WANG Xuerong,YANG Yanghong,YANG Li,CHEN Dapeng,MA Yiqian *Guizhou Provincial Institute of Product Quality Inspection &Testing,Guiyang 550016,

China

[Objectives]To establish a method for determining four tetracycline antibiotics including te -oxytetracycline,and doxycycline in fish meat with ultra performance liquid chro -matography-tandem mass spectrometry (UPLC-MS/MS).[Methods]The samples were extracted with the Na 2EDTA-mcllvaine buffer solution.The grease was removed with -hexane and extracts were purified with Oasis HLB solid phase extraction column.ACQUITY UPLC R BEH C18column (2.1mm ×50mm,

1.7μm)was used to separate four tetracycline antibiotics in fish meat.[Results]Four tetracycline antibi -otics including tetracycline,aureomycin,oxytetracycline,and doxycycline had good linear relationships in the range of 0-100ng/mL,with correlation coefficients ()greater than 0.999.The rates of recovery were all within the range of 70%-120%at the addition level of between 5.0μg/kg and 50.0μg/kg.The rela -tive deviations (RSD)were less than 10%.The limit of detection and quantification of tetracycline an -tibiotics was 5.0，10.0μg/kg,respectively.[Conclusions]The method established can be used for the de -tetracycline antibiotics in fish meat.ultra performance liquid chromatography-tandem mass spectrometry

(UPLC-MS/MS);fish meat;tetracycline;aureomycin;oxytetracycline;doxycycline

试验研究15··

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