超高效液相色谱质谱法快速检测动物源性食品中的四种兽药残留
2012-09-12沙美兰李金强王倩倩关丽丽
沙美兰,曹 鹏,2,*,李金强,王倩倩,关丽丽,牟 妍
(1.烟台出入境检验检疫局,山东烟台 264000;2.山东农业大学食品科学与工程学院,山东泰安271018)
超高效液相色谱质谱法快速检测动物源性食品中的四种兽药残留
沙美兰1,曹 鹏1,2,*,李金强1,王倩倩1,关丽丽1,牟 妍1
(1.烟台出入境检验检疫局,山东烟台 264000;2.山东农业大学食品科学与工程学院,山东泰安271018)
建立了采用超高效液相色谱串联质谱仪快速检测动物组织中甲氧苄胺嘧啶、克林霉素、泰妙菌素和吡喹酮四种药物残留的分析方法。动物组织样品经乙腈提取后,用正己烷去除脂肪等杂质,Waters Acquily UPLC BEH C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,液相色谱-质谱法(UPLCMS/MS)测定。结果表明:4种药物在2.5~200μg/L范围内呈现良好的线性关系,相关系数R2均大于0.996,在此范围内添加回收率为65.8%~95.9%,相对标准偏差为3.2%~13.1%,定量下限为0.5μg/kg。
超高效液相色谱串联质谱,甲氧苄胺嘧啶,克林霉素,泰妙菌素,吡喹酮,动物源性食品
Abstract:An ultra performance liquid chromatography coulped to tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of trimethoprim,clindymycin,tiamulin and praziquantel residues in animal origin food.The sample was extracted with acetonitrile,purified by hexane,and detected on Waters Acquity UPLC BEH C18column by a gradient elution using acetonitrile(A)—0.1%formic acid(B) as mobile phase with a flow rate of 0.3mL/min.The calibration curves were good linear between the peak areas and concentrations of 4 veterinaries in the range of 2.5~200μg/L,with correlation coefficients more than 0.996.The average recoveries at this concentration levels ranged from 65.8%to 95.9%,the RSD was in the range of 3.2%~13.1%.The limits of quantification of 4 drugs in animal origin food were 0.5μg/kg.
Key words:UPLC-MS/MS;trimethoprim;clindymycin;tiamulin;praziquantel;animal original foods
最近,随着食品安全事件的频繁出现,人们对食品安全也愈发的重视,虽然国家对相关药物做了规范,但是在利益的驱使下,还是有不少滥用抗生素的现象。甲氧苄胺嘧啶、泰妙菌素、吡喹酮和克林霉素这四种药物作为抗生素和抗菌素因其特有的效果,目前已经被广泛应用于畜禽类和水产品的养殖中,主要用于防治呼吸系统疾病和寄生虫疾病中等。但是,人们长期食用含有这些药物残留的食物,会对身体健康带来很大的安全隐患。……
