改良QuEChERs-超高效液相色谱-串联质谱法测定羊肉中28种药物残留

Determination of 28 Drug Residues in Lamb by Modified QuEChERs-Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

本研究建立了基于磁性多壁碳纳米管(Fe_(3)O_(4)-MWCNT)的改良QuEChERs法结合超高效液相色谱-串联质谱(UPLC-MS/MS)技术测定羊肉中28种药物多残留的快速、高灵敏检测方法。在优化的色谱及质谱条件下,首先考察不同脱水盐(MgSO_(4)、Na_(2)SO_(4))与金属螯合剂(Na_(2)EDTA)对兽药提取回收率的影响;然后考察Fe_(3)O_(4)-MWCNTs吸附剂的用量对兽药回收率的影响,并与常用的净化材料(C18、PSA、GCB)的净化效果进行比较。结果表明:28种药物在15~500μg/kg浓度范围内的线性关系良好(r~2≥0.999),基质效应低(-9.7%~14.2%),检测限和定量限分别为0.1~5.0μg/kg和0.3~12.0μg/kg;低、中、高(20、100、200μg/kg)3个水平的加标回收率分别为60.2%~114.3%、68.9%~106.7%、60.4%~94.8%;化合物的日内、日间精密度良好,相对标准偏差(RSD)分别不高于9.9%和13.0%。本方法可为动物源食品的安全检测提供更多可能。

Drug abuse is very easy to cause the residues of harmful substances in food of animal origin,which not only does direct harm to human health,but also does great harm to the development of animal husbandry and the ecological environment.Therefore,the detection of residual drugs in animal-derived food is of great significance to ensure food safety.In this study,28 drugs in lambs were simultaneous determined by modified QuEChERs combined with ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) based on magnetic multi-walled carbon nanotubes(Fe_(3)O_(4)-MWCNTs).Under the optimized separation and detection conditions,the effects of different dehydrated salts(MgSO_(4),Na_(2)SO_(4)) and metal chelating agents(Na_(2)EDTA) on the drug recoveries were investigated.Then,the Fe_(3)O_(4)-MWCNTs adsorbent dosages on the purification efficiency were evaluated in terms of drug recoveries and residual matrix masses as well as decoloration effects.The Fe_(3)O_(4)-MWCNTs showed better or equivalent purification performance results than commercial purification adsorbents(C18,PSA,GCB).The results showed that the linear relationship was good for all monitored drugs in the range of 15-500 μg/kg,the correlation coefficient was better than 0.999.By constructing matrix-matched curves and solvent standard curves,the calculated matrix effects(MEs) were located within-9.7%-14.2%,demonstrating its good matrix purification efficiency.Under three spiked concentrations(20,100,200 μg/kg),satisfactory recoveries were obtained in the range of 60.2%-114.3%,68.9%-106.7% and 60.4%-94.8%,respectively,which demonstrated the good accuracy of the method in quantitative analysis.The method precision was validated by intra-and inter-day repetitive experiments on the same day or on the three consecutive days.The obtained intra-and inter-day relative standard deviations(RSDs) were no more than 9.9% and 13.0%,respectively,which indicated the good precision and robustness of the developed method.The limits of detection(LODs) and limits of quantitation(LOQs) were obtained in the range of 0.1-5.0 μg/kg and 0.3-12.0 μg/kg,respectively,which were sensitive enough to analyze the monitored drugs with concentrations exceeding their corresponding maximum residue limits.This method has good applicability in qualitative and quantitative analysis of 28 drug residues in lambs,and can provide a strong technical support for rapid detection of food hazards in other animal origins.