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

Determination of four tetracycline antibiotics in fish meat with ultra performance liquid chromatography tandem mass spectrometry

[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Na2EDTA-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?BEH C18色谱柱(2.1 mm×50 mm,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0-100 ng/mL范围内线性关系良好,相关系数(r)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。

[Objectives]To establish a method for determining four tetracyeline antibiotics including te-tracycline,aureomyein,oxytetracycline,and doxyeycline in fish meat with ultra performance liquid chro-matography-tandem mass spectrometry(UPLC-MS/MS).[Methods]The samples were extracted with the NaEDTA-mellvaine buffer solution.The grease was removed with n-hexane and extracts were purifed with Oasis HLB solid phase extraction column.ACQUITY UPLC■BEH C18 column(2.1 mm×50 mm,1.7μm)was used to separate four tetracyeline antibiotics in fish meat.[Results]Four tetracyeline antibi-otics including tetracyeline,aureomyein,oxytetracyeline,and doxycyeline had good linear relationships in the range of 0-100 ng/mL,with correlation coefficients(r)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-termination of tetracyecline antibiotics in fish meat.