超高效液相色谱-串联质谱法测定牛奶中三氮脒残留  

Determination of diminazene in milk by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：张璐 董立雅 刘通 聂雪梅[1,4] 许博舟 许秀丽[1,4] 逯刚 ZHANG Lu;DONG Li-Ya;LIU Tong;NIE Xue-Mei;XU Bo-Zhou;XU Xiu-Li;LU Gang(Institute of Food Safety,Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123,China;Inner Mongolia Meng-Niu Dairy(Group)Co.,Ltd.,Hohhot 011500,China;Chinese Academy of Inspection and Quarantine,Key Laboratory of Food Quality and Safety for State Market Regulation,Beijing 100176,China)

机构地区：[1]中国检验检疫科学研究院,食品安全研究所,北京100176 [2]重庆市计量质量检测研究院,重庆401123 [3]内蒙古蒙牛乳业(集团)股份有限公司,呼和浩特011500 [4]中国检验检疫科学研究院,国家市场监管重点实验室(食品质量与安全),北京100176

出　　处：《食品安全质量检测学报》2024年第11期45-52,共8页Journal of Food Safety and Quality

基　　金：国家市场监督管理总局科技创新人才计划(青年拔尖人才)项目(QNBJ202322)。

摘　　要：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)检测牛奶中痕量三氮脒残留的分析方法。方法样品采用1%乙酸乙腈溶液振荡提取后,在–4℃条件下高速离心,取上清液旋转蒸干,以10%乙腈水溶液复溶,用UPLC-MS/MS检测。采用BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,以乙腈-0.1%甲酸水溶液作为流动相梯度洗脱,流速为0.2 mL/min,在正离子扫描及多反应监测(multiple reaction monitoring,MRM)模式下分析,外标法定量。结果牛奶中三氮脒的检出限(limit of detection,LOD)为5μg/kg,定量限(limit of quantification,LOQ)为15μg/kg,在20~1000μg/L质量浓度范围内线性良好,相关系数(r)为0.9993。将所研究的方法应用于实际牛奶样本中,其日内加标回收率在81.67%~85.49%,日内精密度在4.5%~5.5%,日间加标回收率在81.07%~85.12%,日间精密度在5.9%~8.2%。结论本方法采用振荡提取加低温高速离心净化的前处理方法,简单快速,结合UPLC-MS/MS,可实现痕量水平残留的高灵敏度检测,适用于牛奶中的三氮脒残留的快速检测,为动物源性食品中三氮脒残留的定性与定量分析提供技术参考。Objective To establish a method for the determination of trace diminazene residues in milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Samples were extracted by oscillation with 1%acetic acid-acetonitrile,after high-speed centrifugation at–4℃,the liquid supernatant was dried by rotary evaporation and dissolved with 10%acetonitrile aqueous solution,and determined by UPLC-MS/MS.A BEH C18 column(100 mm×2.1 mm,1.7μm)was used for separation,and acetonitrile-0.1%formic acid aqueous solution was used as mobile phase for gradient elution,the elution flow rate was 0.2 mL/min.The positive ion scanning mode and multiple reaction monitoring(MRM)was used,and the external standardization method was used for the quantitative analysis.Results The limit of detection(LOD)and limit of quantification(LOQ)of diminazene in milk were 5μg/kg and 15μg/kg,respectively.In the mass concentration range of 20–1000μg/L,the linearity was good,with a correlation coefficient(r)of 0.9993.The recoveries ranged from 81.67%to 85.49%(intra-day)and 81.07%to 85.12%(inter-day)when applied in milk detection,with intra-day precisions of 4.5%–5.5%and inter-day precisions of 5.9%–8.2%.Conclusion This method adopts a pretreatment method of oscillation extraction and low-temperature high-speed centrifugation purification,which is simple and fast.By incorporating UPLC-MS/MS,high sensitivity detection of trace residues can be attained,making it suitable for the rapid detection of triazamidine residues in milk,providing technical reference for the qualitative and quantitative analysis of diminazene residues in animal derived foods.

关 键 词：三氮脒 牛奶 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]