食品中99种兽药的一步式提取净化体系
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摘要
建立了99种禁限用兽药的一步式提取净化体系,并通过高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q-Orbitrap HRMS)对其效果进行了评价。该提取净化体系基于载体辅助液液萃取技术,通过一次性前处理,完成常见的理化性质差异很大的8大类共计99种兽药残留的提取、净化工作,同时结合四极杆静电场轨道阱高分辨质谱实现了99种兽药残留的一步式多残留筛查。采用此体系对样品禁限用兽药进行测定分析,结果表明,该方法对液态乳、猪肉、鱼类等食品基质具有较强的适用性,检测的99种兽药线性范围为0.001~0.1μg/m L,定量限为0.5~20.0μg/kg,加标回收率为60%~120%,相对标准偏差小于15%。该方法的前处理和仪器分析过程对不同理化性质的化合物的兼容性强,检测效率高,可操作性强,检出限能满足所有受试的目标物,并且大大降低了检测成本。
We established a system for the simultaneous extraction and cleaning of 99 veterinary drugs from food by ultra-performance liquid chromatography coupled with quadrupole electrostatic field-orbital trap-high-resolution mass spectrometry( UHPLC-Q-Orbitrap HRMS). The system is based on the supported liquid-liquid extraction technology through one-off pretreatment,which covers the common eight categories of physical and chemical properties,and the extraction and purification of 99 different veterinary drug residues. At the same time,the onestep multi residue screening of 99 veterinary drug residues has been realized using HRMS. The results showed that the method was suitable for extraction from milk,pork,and fish. The 99 veterinary drugs showed a good linear relationship in the concentration range of 0. 001-0. 1μg/mL,the limit of quantification was 0. 5-20. 0 μg/kg,the average recoveries were 60%-120%,and the relative standard deviations( RSDs) were not more than 15%. The preprocessing and instrumental analysis of this method have high detection efficiency,strong maneuver ability,and strong compatibility with different physical and chemical compounds. Moreover,the detection limit can meet all the objects of the test and greatly reduce the detection cost.
We established a system for the simultaneous extraction and cleaning of 99 veterinary drugs from food by ultra-performance liquid chromatography coupled with quadrupole electrostatic field-orbital trap-high-resolution mass spectrometry( UHPLC-Q-Orbitrap HRMS). The system is based on the supported liquid-liquid extraction technology through one-off pretreatment,which covers the common eight categories of physical and chemical properties,and the extraction and purification of 99 different veterinary drug residues. At the same time,the onestep multi residue screening of 99 veterinary drug residues has been realized using HRMS. The results showed that the method was suitable for extraction from milk,pork,and fish. The 99 veterinary drugs showed a good linear relationship in the concentration range of 0. 001-0. 1μg/mL,the limit of quantification was 0. 5-20. 0 μg/kg,the average recoveries were 60%-120%,and the relative standard deviations( RSDs) were not more than 15%. The preprocessing and instrumental analysis of this method have high detection efficiency,strong maneuver ability,and strong compatibility with different physical and chemical compounds. Moreover,the detection limit can meet all the objects of the test and greatly reduce the detection cost.
引文
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[3]Yan H,Yun H,Liu X.Journal of Instrumental Analysis,2013,32(8):909严华,云环,刘鑫.分析测试学报,2013,32(8):909
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[5]Li F G,Su M,Li X Y.Chinese Journal of Chromatography,2011,29(2):120李锋格,苏敏,李晓岩.色谱,2011,29(2):120
[6]Wang L,Li Y Q,Wang H B.Chinese Journal of Analytical Chem istry,2011,39(2):203王炼,黎源倩,王海波.分析化学,2011,39(2):203
[7]Wang C Y,Wang Y P,Wang N.Chinese Journal of Analytical Chem istry,2013,41(1):83王重洋,王远鹏,王宁.分析化学,2013,41(1):83
[8]Xi J Z,Song J,Wang G N.Heilongjiang Animal Science and Veterinary Medicine,2015(1):53锡建中,宋娇,王庚南.黑龙江畜牧兽医,2015(1):53
[9]Chen S B,Shan Z J,Hu Q H.Food Science,2004(12):152陈树兵,单正军,胡秋辉.食品科学,2004(12):152
[10]Yu J.[MS Dissertation].Hubei:Huazhong Agricultural University,2012于洁.[博士学位论文].湖北:华中农业大学,2012
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[12]Qu B.Food Science,2013,34(5):327曲斌.食品科学,2013,34(5):327
[13]Quintana J B,Rodriguez I.Anal Bioanal Chem,2006,384:1447
[14]Li X W,Guo P,Shan Y W,et al.J Chromatogr A,2017,1499(26):57
[15]Gao F D,Zhao Y,Shao B,et al.Chinese Journal of Chrom ato graphy,2012,30(6):560高馥蝶,赵妍,邵兵,等.色谱,2012,30(6):560
[16]Chu X G,Yong W,Ling Y,et al.Chinese Journal of Chrom ato graphy,2007,25(6):907储晓刚,雍炜,凌云,等.色谱,2007,25(6):907
[17]Zhao Y S,Yang M L,Zhang F,et al.Chinese Journal of Chro m ato graphy,2011,29(7):631赵延胜,杨敏莉,张峰,等.色谱,2011,29(7):631
[18]Didier O,Emmanuelle C,Philippe J,et al.J Chromatogr B,2009,877(23):2363
[19]Chepyala D,Tsaide I L,Liao H W,et al.J Chromatogr A,2017,1491(31):57