摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定牛奶中9种兽药和10种新烟碱类农药残留的方法。方法样品用1%甲酸乙腈:乙二胺四乙酸二钠盐-磷酸盐缓冲液(ethylene diamine tetraacetic acid disodium salt-Mcllvaine,Na2EDTA-Mcllvaine)(8:2,V:V)溶液提取,十八烷基硅烷(C18)净化,采用Waters ACQUITYUPLC■BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,以5 mmol/L甲酸铵(含0.1%甲酸,V:V)和甲醇(含0.1%甲酸,V:V)为流动相梯度洗脱,在质谱电喷雾电离源(electrospray ionization,ESI),正离子源条件下,以多反应监测(multiple reaction monitoring,MRM)模式采集检测,基质匹配标准曲线外标法定量。结果19种目标物线性关系良好(相关系数r>0.9990),检出限和定量限分别为0.05~0.90μg/kg和0.17~3.00μg/kg。空白样品在10、20和50μg/kg加标水平下,目标物的回收率为62.5%~109.7%,相对标准偏差为2.4%~9.8%(n=6)。结论该方法简单快速,能满足牛奶中多种兽药和新烟碱类农药残留的同时快速筛查。
Objective To establish an analytical method for the simultaneous determination of 9 kinds of veterinary drug and 10 kinds of neonicotinoid pesticide residues in milk by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted with a solution of 1% formic acid acetonitrile and ethylene diamine tetraacetic acid disodium salt-Mcllvaine,Na2EDTA Mcllvaine buffer with a volume ratio of 8:2(V:V).The extract was purified by C18,and the separation was completed on a Waters ACQUITY UPLC■BEH C_(18) column(2.1 mm×100 mm,1.7μm)with a gradient system of mixture of 5 mmol/L ammonium formate and methanol with 0.1% formic acid(V:V)solution as mobile phase.The samples were scanned simultaneously under the conditions of mass spectrometry electrospray ionization(ESI)and positive ion sourcemode,detected in multiple reaction monitoring(MRM)mode,and quantified by matrix matching curve external standard method.Results The linear relationships of 19 kinds of compounds were good,with the correlation coefficients(r)greater than 0.9990,and the limits of detection and limits of quantitation were in the ranges of 0.05-0.90μg/kg and 0.17-3.00μg/kg,respectively.The average recoveries were 62.5% to 109.7% with relative standard deviations of 2.4% to 9.8%(n=6)at 3 spiked levels(10,20 and 50μg/kg).Conclusion This method is simple and fast,and can quickly screen for various veterinary drug and neonicotinoid pesticide residues in milk.
作者
张敏
唐彬彬
刘峰
宋丽新
贺敏
程静
ZHANG Min;TANG Bin-Bin;LIU Feng;SONG Li-Xin;HE Min;CHENG Jing(Baotou Center for Disease Control and Prevention,Baotou 014030,China)
出处
《食品安全质量检测学报》
2025年第22期152-159,共8页
Journal of Food Safety and Quality
关键词
QUECHERS
超高效液相色谱-串联质谱法
牛奶
兽药残留
新烟碱类农药残留
QuEChERS
ultra performance liquid chromatography-tandem mass spectrometry
milk
veterinary drug residues
neonicotinoid pesticide residues
