液-质联用法同时检测植物源性食品中4种鼠药残留
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摘要
建立液相色谱-质谱联用仪测定植物源性食品中4种鼠药残留的方法。考察不同的流动相及净化方式对检测结果的影响。粮谷类试样经乙腈超声提取上机,果蔬类以乙腈提取后采用PSA+GCB管进行净化,LC/MS-MS进行检测。添标水平为0.002~0.050mg/kg时的回收率均达到70%以上,相对标准偏差为4.1%~9.5%,杀鼠醚和杀鼠灵的方法检出限为0.001mg/kg,其它2种鼠药的检出限为0.005mg/kg。该方法快速、简单、灵敏度高,符合GB/T 27404—2008对方法确认技术参数的要求。
To establish a LC/MS-MS method for determination of 4 kinds of rodenticide residues in plant-origin food,the effects of different mobile phase and purification on the recovery was studied.The grain samples were extracted by acetontrile and then determined by LC/MS-MS,while the samples with fruit or vegetable matrix were purified with PSA+GCB after the extraction.LC/MS-MS was used for determination.The recoveries were all above 70% at spiked levels of 0.002~0.050 mg/kg,and the relative standard deviation of the methods were 4.1%~9.5%.The LOD of warfarin and coumatetralyl were 0.001 mg/kg while the other two reach 0.005 mg/kg which was in accordance with the requirement of technical parameters for analysis,with fast and simple determination and high sensitivity.
To establish a LC/MS-MS method for determination of 4 kinds of rodenticide residues in plant-origin food,the effects of different mobile phase and purification on the recovery was studied.The grain samples were extracted by acetontrile and then determined by LC/MS-MS,while the samples with fruit or vegetable matrix were purified with PSA+GCB after the extraction.LC/MS-MS was used for determination.The recoveries were all above 70% at spiked levels of 0.002~0.050 mg/kg,and the relative standard deviation of the methods were 4.1%~9.5%.The LOD of warfarin and coumatetralyl were 0.001 mg/kg while the other two reach 0.005 mg/kg which was in accordance with the requirement of technical parameters for analysis,with fast and simple determination and high sensitivity.
引文
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[15]朱峰,刘华良,陈蓓,等.超高效液相色谱-串联质谱法同时快速筛查检测食品中的10种抗凝血类鼠药[J].色谱,2013(5):473-476.
[16]董静,潘玉香,朱莉萍,等.果蔬中54种农药残留的QuEChERS/GC-MS快速分析[J].分析测试学报,2008,27(1):66-69.
[17]KOMASAWA N,UEKI R,KAMINOH Y,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1 217(16):2 548-2 560.
[2]广跃乾,王琼,刘厚鹏,等.大剂量维生素K1救治抗凝血灭鼠药中毒19例治疗体会[J].北方药学,2012,9(6):110-110.
[3]谷日旭,王彩云,米尔芳.紫外分光光度法测定中毒样品中敌鼠含量[J].实用医技杂志,2010,17(4):338-338.
[4]麦沛明,余胜兵,吴西梅,等.分散液-液微试剂-气相色谱-质谱法同时测定中毒样品中有毒生物碱和鼠药[J].分析化学,2015(2):282-287.
[5]李文海,朱鲁生.固相萃取GC/MS分析血中10种常见农药和杀鼠药[J].中国法医学杂志,2009,24(4):269-271.
[6]王洪宗,冯辉,胡开发,等.GC/ECD法测定生物检材中溴敌隆和大隆[J].中国法医学杂志,2008,23(6):405-406.
[7]贺燕,徐文泱,孙桂芳,等.气相色谱-质谱法检测肉制品中的杀鼠酮[J].食品与机械,2017,33(5):99-102.
[8]陈晓红,蔡美强,金米聪.高效液相色谱/离子阱质谱快速鉴定茚满二酮类鼠药[J].卫生研究,2010,39(5):586-590.
[9]MIDDLEBERG R A,HOMAN J.Qualitative identification of rodenticide anticoagulants by LC-MS/MS[J].Methods in Molecular Biology,2012,902:139-148.
[10]孟庆玉,黎源倩,邹晓莉,等.浊点试剂-高效液相色谱法同时测定人尿中的4种抗凝血鼠药[J].分析化学,2008,36(6):760-764.
[11]陈晓红,金米聪.采用液相色谱-串联质谱法检测血清中痕量异杀鼠酮[J].中华预防医学杂志,2010,44(11):1 060-1 062.
[12]HERNANDEZ A M,BERNAL J,BERNAL J L,et al.Analysis of anticoagulant rodenticide residues in Microtus arvalis tissues by liquid chromatography with diode array,fluorescence and mass spectrometry detection[J].Journal of Chromatography B,2013,925:76-85.
[13]ZHU Lin,YAN Hui,SHEN Bao-hua,et al.Determination of bromadiolone and brodifacoum in human hair by liquid chromatography/tandem mass spectrometry and its application to poisoning cases[J].Rapid Communications in Mass Spectrometry,2013,27(4):513-520.
[14]麦沛明,余胜兵,吴西梅,等.分散液-液微试剂-气相色谱-质谱法同时测定中毒样品中有毒生物碱和鼠药[J].分析化学,2015(2):282-287.
[15]朱峰,刘华良,陈蓓,等.超高效液相色谱-串联质谱法同时快速筛查检测食品中的10种抗凝血类鼠药[J].色谱,2013(5):473-476.
[16]董静,潘玉香,朱莉萍,等.果蔬中54种农药残留的QuEChERS/GC-MS快速分析[J].分析测试学报,2008,27(1):66-69.
[17]KOMASAWA N,UEKI R,KAMINOH Y,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1 217(16):2 548-2 560.