高效液相色谱-电喷雾-iFunnel-串联质谱法同时测定猪尿液中20种禁用兽药残留

Simultaneous Determination of 20 Forbidden Veterinary Drug Residues in Swine Urine by HPLC- ESI- iFunnel- MS / MS

建立了一种猪尿液中20种禁用兽药的高效液相色谱-电喷雾-iFunnel-串联质谱（HPLC-ESI-iF-unnel-MS/MS）检测方法.尿液样品直接经HLB固相萃取柱净化,甲醇洗脱,氮气吹干后,用乙腈-水（1：9,体积比）定容至1 mL.待测物采用Eclipse Plus C18柱进行分离,串联四极杆质谱进行检测,以电喷雾正离子模式（ESI＋）扫描,iFunnel离子聚焦,多反应离子监测,外标法定量.结果显示,在0.1～ 50 μg/L浓度范围内,20种兽药的线性系数均大于0.99,检出限（LOD）为0.05～0.2 μg/L,定量下限（LOQ）为0.1～0.5 μg/L.在3个加标水平下20种药物的平均回收率为81.5％ ～ 104.8％,相对标准偏差为3.0％ ～16.0％.采用该方法对养殖户及实验室采集的猪尿液样品进行分析,20种禁用药物均未检出.本方法快速、灵敏、高通量,能满足国内外20种禁用兽药残留限量的检测要求.

An HPLC-ESI-iFunnel-MS/MS method was established for the simultaneous determination of 20 forbidden veterinary drugs in swine urine.The urine matrix was directly purified by HLB solid phase extraction cartridges and blown dry with nitrogen after eluted with methanol,then redissolved with acetonitrile-water（1 ∶ 9,by volume） to 1 mL.The target compound was separated on an Eclipse Plus C18 column and detected by MS/MS under electrospray ionization in positive ion mode.The iFunnel technology was used to focus ions and multiple reaction monitoring （MRM） was used to monitor ions.Standard curve method was used for quantitative analysis.Good linearities of 20 forbidden veterinary drugs were observed in the range of 0.1-50 μg/L with correlation coefficients higher than 0.99.The average recoveries at three spiked concentration levels ranged from 81.5％ to 104.8％,with relative standard deviations （RSDs） of 3.0％-16.0％.The limits of detection （LOD） were in the range of 0.05-0.2 μg/L and the limits of quantitation（LOQ） were 0.1-0.5 μg/L.The established method was used for the determination of 20 forbidden veterinary drugs in real urine samples collected from a farm and laboratory,and none of the 20 forbidden veterinary drugs was detected.With the advantages of rapidness,sensitivity and high throughput,this method could meet the requirements for residue limits detection at home and abroad.