同位素内标-超高效液相色谱串联质谱法测定禽类食品中喹诺酮与四环素残留量
目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定禽类食品中11种喹诺酮与4种四环素兽药残留的方法。方法 鸡肉和鸡蛋样品经Mcllvaine-Na2EDTA缓冲液提取, 7%钨酸钠溶液沉淀蛋白, HLB柱净化, 喹诺酮类药物采用10 mmol/L乙酸铵(含0.1%甲酸, V:V)与甲醇为流动相, 四环素类药物采用0.1%甲酸与乙腈为流动相。2种类型药物均采用多反应监测模式监测, 内标法定量。结果 15种兽药残留在0.1~50.0 μg/L的浓度范围内线性良好, 相关系数均大于0.9927, 检出限为0.05~0.20 μg/kg, 平均回收率为60.6%~117.9%, 相对标准偏差为0.51%~15.3%。采用建立的方法检测安徽省市售2016~2018年的鸡肉和鸡蛋样品中喹诺酮与四环素残留, 检测结果通过食品安全指数(international foundation for science, IFS)评估, 发现鸡肉和鸡蛋中喹诺酮类IFS均值分别为0.00048、0.000097 μg/(kg?bw?d), 四环素类IFS均值分别为0.00073、0.00098 μg/(kg?bw?d), 均小于1, 说明其膳食暴露风险较低。结论 该方法的样品前处理可以完全沉淀蛋白, 净化效果好, 能够减少基质效应的影响, 适用于大批量禽类食品中喹诺酮与四环素兽药残留量的快速测定。
Objective To establish a method for the determination of 11 quinolones and 4 tetracycline residues in animal products from poultry by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The analysts were extracted from the chicken and egg samples using the Mcllvaine-Na2EDTA buffer solution. The protein in extract was precipitated by 7% sodium tungstate solution, and then the extract was purified on the HLB column. The quinolones were detected using the methanol and 10 mmol/L ammonium acetate (containing 0.1% formic acid, V:V) as the mobile phases. The tetracyclines were detected using the acetonitrile and 0.1% formic acid (V:V) as the mobile phases. Both types of drugs were monitored by multiple reactions monitoring mode and quantified by the internal standard method. Results The 15 veterinary drug residues had good linearity in the concentration range of 0.1?50.0 μg/L, the correlation coefficients were all greater than 0.9927, the limits of detections were 0.05?0.20 μg/kg, the average recoveries were 60.6%?117.9%, and the relative standard deviations were 0.51%?15.3%. The established method was used to detect the residues of quinolone and tetracycline in chicken and egg samples sold in Anhui province from 2016 to 2018. The test results were evaluated by the international foundation for science (IFS), and it was found that the average IFS of quinolones in chicken and eggs were 0.00048 and 0.000097 μg/(kg?bw?d), respectively, and the mean values of tetracycline IFS were 0.00073 and 0.00098 μg/(kg?bw?d), respectively, which were both less than 1, indicating that their dietary exposure risks were low. Conclusion This method can completely precipitate the protein, has good purification effect, and can reduce the influence of matrix effect. It is suitable for the rapid determination of quinolones and tetracycline residues in large quantities of poultry food.
标题：同位素内标-超高效液相色谱串联质谱法测定禽类食品中喹诺酮与四环素残留量
英文标题：Determination of quinolones and tetracycline residues in poultry food by isotope internal standard-ultra performance liquid chromatography-tandem mass spectrometry
作者：
刘柏林 安徽省疾病预防控制中心
谢继安 安徽省疾病预防控制中心
赵紫微 安徽省疾病预防控制中心
单晓梅 安徽省疾病预防控制中心
王秀莉 安徽省疾病预防控制中心
中文关键词:超高效液相色谱-串联质谱法,喹诺酮,四环素,鸡蛋,鸡肉,同位素内标,
英文关键词:ultra performance liquid chromatography-tandem mass spectrometry,quinolones,tetracycline,eggs,chicken,isotopic internal standard,
发表日期：2020-06-12
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