HPLC-Q-TOF法筛查鸡肉中48种兽药残留

Screening and Determination of 48 Veterinary Drug Residues in Chicken by High Performance Liquid Chromatography/Quadrupole Time of Flight Mass Spectrometry

利用高效液相色谱-四级杆-飞行时间质谱(UPLC-Q-TOF/MS)建立了鸡肉中48种兽药残留的快速筛查和检测方法。样品采用乙腈/水(7∶3,体积比)提取,经Oasis PRi ME HLB固相萃取柱净化,采用UPLC-Q-TOF/MS检测,正离子全信息串联质谱模式扫描,外标法定量。建立了目标分析物一级精确质量数据库和谱图库,通过化合物的精确质量数、保留时间等对检测结果进行检索,从而在无对照标准品的情况下可以对目标分析物进行定性鉴定。结果表明,鸡肉中48种兽药的定量限(LOQ,S/N=10)为3.0μg/kg^30μg/kg,在3.0μg/L^300μg/L范围呈良好线性,线性相关系数均大于0.99。该方法灵敏、简便、准确,可用于鸡肉中多种兽药残留的检测分析。

An analytical method was established for the simultaneous determination of 48 veterinary drug residues in chicken by high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF/MS). The samples was extracted with acetonitrile and water(7∶3,volume ratio),and determined by UPLC-Q-TOF/MS after cleaned-up by solid phase extraction with a Oasis PRi ME HLB cartridge. The target compounds was quantified by external standard method with acquisition under positive ion mode was performed to obtain accurate relative molecular masses. A date base containing the accurate mass numbers and a library which contains the 48 veterinary drugs were established. According to the characteristics of accurate mass,retention time and so on,the qualitative identifications of 48 veterinary drugs were accomplished without the contrast of standard substances. The results showed that the calibration curves were linear in the range of 3.0 μg/L-300 μg/L for 48 veterinary drugs with correlation coefficient(r)more than 0.99. The lim its of quantitation(LODs,S/N=10)were in the range of 3.0 μg/kg-30 μg/kg. The method was sensitive,convenient and accurate,and could satisfy the demand of detection and analysis of veterinary drug residues in chicken.