摘要
建立了超高效液相色谱-四极杆-飞行时间质谱快速筛查牛奶中β-受体激动剂类、磺胺类、喹诺酮类、四环素类4类共69种兽药残留量的分析方法。牛奶用含0.5%甲酸的乙腈溶液提取,乙腈饱和的正己烷净化除脂,使用ACQUITY UPLC BEH C_(18)色谱柱分离,以0.1%甲酸和含0.1%甲酸的甲醇-乙腈(2∶8)为流动相梯度洗脱,10 min内可实现69种兽药的良好分离,在电喷雾离子源(ESI)正离子模式下运用全扫描和数据依赖采集(DDA)方式进行测定。牛奶中69种兽药的定量下限(LOQ)为10µg·kg^(-1);在10、50、100µg·kg^(-1)下的平均加标回收率为59.0%~120%,相对标准偏差(RSD)为0.80%~13%。该方法操作简单,检测效率高,可用于牛奶中69种兽药的快速筛查。
An ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method was developed for rapid screening of 69 veterinary drugs belonging to four classes(β-agonists,sulfonamides,quinolones and tetracyclines)in milk.The extraction was per-formed using acetonitrile solution containing 0.5%formic acid,and the purification was carried out by liquid-liquid extraction using n-hexane for defatting.An ACQUITY UPLC BEH C_(18) column was used for chromatographic separation,and gradient elution was performed using 0.1%formic acid and methanol-acetonitrile(2∶8)containing 0.1%formic acid as the mobile phases.The electrospray ion-ization was used in positive ion mode for full scan and data-dependent acquisition mode(DDA)detec-tion.Efficient separation of 69 veterinary drugs can be achieved within 10 min.The limits of quantifi-cation(LOQs)of 69 veterinary drugs in milk was 10µg·kg^(-1).The average recoveries was 59.0%-120%with relative standard deviations(RSDs)of 0.80%-13%at three spiked levels(10,50 and 100µg·kg^(-1)).This method is simple and efficient,and can be used for the rapid screening of 69 veterinary drugs in milk.
作者
严祖浩
李晓薇
夏曦
YAN Zu-hao;LI Xiao-wei;XIA Xi(College of Veterinary Medicine,China Agricultural University,Beijing 100193,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第10期1309-1318,共10页
Journal of Instrumental Analysis
关键词
牛奶
超高效液相色谱
飞行时间质谱
兽药残留
快速筛查
milk
ultra-high performance liquid chromatography
time-of-flight mass spectrome-try
veterinary drug residues
rapid screening
