超高效液相色谱串联质谱法同时分析饲料中29种兽药

建立一种同时测定饲料中29种兽药残留的超高效液相色谱串联质谱分析方法。样品经甲醇-乙腈混合溶液（1＋1）提取和Oasis HLB固相萃取柱净化,采用C18色谱柱（2.1mm×50mm,1.7μm）分离,以甲醇和0.2%甲酸水溶液作为流动相进行梯度洗脱,UPLC-MS/MS法同时定性、定量测定喹诺酮类、磺胺类、大环内酯类、硝基呋喃类共计29种兽药残留。29种兽药在0.01-5.0μg/mL范围内线性关系良好,相关系数（r2）均大于0.99;以0.01mg/kg,0.05mg/kg,0.5mg/kg,2.0mg/kg 4个浓度水平进行添加回收实验,29种药物平均回收率72.2%-94.9%,相对标准偏差2.03%-13.23%,方法检出限为0.01mg/kg或0.05mg/kg。方法重现性、灵敏度高、分析时间短、确证能力强,适用于饲料中29种兽药残留的同时检测。

Simultaneous analysis of 29 veterinary drugs residues in feed by ultra performance liquid chromatography-mass spectrometry

A confirmative method of ultra performance liquid chromatography-mass spectrometry（UPLC-MS） for the simultaneous determination of 29 veterinary drugs residues in feed was developed.The sample was extracted with methanol and acetonitrile solution（1＋1） and purified by an Oasis HLB solid phase extraction cartridge.The UPLC separation was performed on an C18 column（2.1mm×50mm,1.7μm） utilizing a gradient elution program of methanol and water（containing0.2%formicacid） as the mobile phase.The identification and quantification of 29 veterinary drugs residues of quinolones,sulfonamides,macrolides,nitrofuranwere achieved by using UPLC-MS/MS.The linear ranges were from 0.01~5.0 μg/mL with the correlation coefficients above 0.99 for all the 29 veterinary drugs.The average recoveries spiked at the 4 concentration levels of 0.01mg/kg,0.05mg/kg,0.5mg/kg,2.0 mg/kg ranged from 72.2% to 94.9% with the relative standard deviations of 2.03%~13.23%.The limits of detection were 0.01mg/kg or 0.05mg/kg.The method was proved to be good reproducibility,high sensitivity,rapid,reliable and suitable for thesimultaneous determination of multi-residues of 29 veterinary drugs residues in feed.