超高效液相色谱串联四极杆飞行时间质谱快速筛查猪肉中29种抗菌药物的残留
Rapid screening of 29 kinds of antibacterial drugs in pork by UPLC- Q- TOFMS
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摘要: 采用超高效液相色谱串联四极杆飞行时间质谱仪（UPLC-Q-TOFMS）建立了猪肉中磺胺、喹诺酮、大环内酯、林可酰胺等4类29种抗菌类药物残留的筛查数据库;并结合快速高通量的前处理方法实现了猪肉中抗菌类药物的快速筛查测定。样品经Mcllvaine缓冲液提取,HLB固相萃取柱净化,采用BEH C18 UPLC色谱柱分离,梯度洗脱,采用全信息串联质谱扫描模式（MSE）进行检测,精确质量数的母离子定量。结果表明:29种抗菌药物的定量限（LOQ,S/N≥10）为0.510μg/kg,高、中、低3个添加水平平均回收率为50.10%118.33%,相对标准偏差（RSD）为0.31%14.90%,该方法能够达到高通量、多组分、快速开放的筛查目的,可用于猪肉基质中抗菌药物的批量快速筛查工作。Abstract: A screening database for 29 kinds of antibacterial drugs including sulfonamides,fluoroquinolones,macrolides and lincosamides in meat was established by ultra-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry. Combined with a rapid high throughput pretreatment,it can fast screen and test the antibacterial drugs in pork.Samples were extracted by Mcllvaine buffer and cleaned up by HLB solid phase extraction tube.Chromatography method was separated by BEH C18 UPLC column,eluted whit gradient solvent,detected by MSE acquisition and quantitative by parent ion with exact mass. The result showed that the LOQs of 29 antibacterial drugs in matrixes were between 0.5 μg/kg and 10 μg/kg.Average recoveries in 3 different spiked levels were 50.10% ~118.33%,RSD were 0.31% ~14.90%.This method can achieve a high throughput,multicomponents,rapid and open screening and appropriate in rapid screening antibacterial drugs in pork.
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