摘要
目的 建立固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时检测禽蛋中12种禁用兽药残留的方法。方法 样品经1.0%甲酸乙腈提取,经PRiME HLB固相萃取柱净化,氮气浓缩至近干后,残渣用流动相溶解,目标物用ACQUITY UPLC^(?)HSS T3色谱柱(50 mm×2.1 mm,1.8μm)分离,以乙腈和0.02%甲酸+5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,内标法定量。结果 12种兽药在0.50~300.00μg/L范围内线性关系良好,相关系数均大于0.99,检出限为0.05~1.50μg/kg,定量限为0.10~3.00μg/kg。加标回收率为80.02%~114.24%,相对标准偏差为2.09%~15.03%。结论 该方法 前处理简单、准确、成本较低,适用于禽蛋中兽药残留的高通量快速检测分析。
Objective To establish a method for simultaneous determination of 12 kinds of banned veterinary drug residues in poultry eggs by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample was extracted by 1.0% formic acid acetonitrile,and purified by the PRIME HLB solid phase extraction column.After concentrated to near dry with nitrogen,the residue was dissolved by mobile phase,and the target was separated with an ACQUITY UPLC?HSS T3 column(50 mm×2.1 mm,1.8 μm) using acetonitrile and 0.02% formic acid+5 mmol/L ammonium acetate aqueous solution as mobile phase for gradient elution,quantified by the internal standard method.Results The 12 kinds of veterinary drugs had good linear relationships in the range of 0.50–300.00 μg/L,and the correlation coefficients were greater than 0.99,the limits of detection were 0.05–1.50 μg/kg,the limits of quantification were 0.10–3.00 μg/kg.The adding standard recoveries were 80.02%– 114.24%,and the relative standard deviations were 2.09%–15.03%.Conclusion The method is simple,accurate and low-cost,and is suitable for the rapid determination of veterinary drugs residues in poultry eggs with high throughput.
作者
秦宇
葛宇
QIN Yu;GE Yu(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第7期2258-2266,共9页
Journal of Food Safety and Quality
基金
上海市质量监督检验技术研究院项目(KY-2020-9-SP)
上海市科技创新行动计划技术标准项目(19DZ2202400)。
关键词
超高效液相色谱-串联质谱法
固相萃取
兽药残留
禽蛋
ultra performance liquid chromatography-tandem mass spectrometry
solid phase extraction
veterinary drugs residues
poultry eggs
