当归中禁限用农药多残留检测方法的建立
|
摘要
建立当归50种农药多残留的液相色谱-串联质谱(LC-MS/MS)检测方法,并应用于182批次样品初步筛查。依据风险控制的基本原则选择我国禁限用、高毒、高风险及当归种植中常用的农药品种为检测指标。对样品前处理方法、色谱质谱条件都进行了优化,最终经乙腈提取、以液相色谱分离,在串联质谱多反应监测(MRM)模式下测定。并采用内标法计算以提高结果的准确性。以当归为考察对象,该方法在1～100μg·L~(-1)线性良好,相关系数R2> 0. 990,3水平加标回收率试验中93. 9%以上农药平均回收率在60%～140%,符合痕量测定的要求。该方法以我国常用大宗药物当归为研究对象,有针对性地检测了当归中高风险、高毒性的农药品种,涵盖了绝大多数禁限用农药,检测方法快速、准确,适用于农药残留风险监测和日常检测。
The present study is to establish a method for simultaneous determination of 50 kinds of pesticides in Angelicae Sinensis Radix by using liquid chromatography tandem mass spectrometry. The forbidden,restricted and customary pesticides were picked out as detecting indexes according to the principals of risk management. The factors affecting the extraction,purification,and detection were optimized,and the final condition was established as follows: the samples were extracted with acetonitrile. The separation of target compounds were performed by liquid column,and quantitative analysis was carried out by LC-MS/MS with MRM model. The calibration curves were linear in the range of 1-100 μg·L~(-1) with correction coefficients of greater than 0. 990. The recoveries of more than 93. 9%pesticides were ranged from 60% to 140% at three spiked levels. The detecting indexes in the method cover most forbidden and restricted pesticides,which is meaningful for the safety supervision of the Angelicae Sinensis Radix. With the advantage of rapidness and accuracy,this method can be used for routine determination of multi-pesticides in Angelicae Sinensis Radix.
The present study is to establish a method for simultaneous determination of 50 kinds of pesticides in Angelicae Sinensis Radix by using liquid chromatography tandem mass spectrometry. The forbidden,restricted and customary pesticides were picked out as detecting indexes according to the principals of risk management. The factors affecting the extraction,purification,and detection were optimized,and the final condition was established as follows: the samples were extracted with acetonitrile. The separation of target compounds were performed by liquid column,and quantitative analysis was carried out by LC-MS/MS with MRM model. The calibration curves were linear in the range of 1-100 μg·L~(-1) with correction coefficients of greater than 0. 990. The recoveries of more than 93. 9%pesticides were ranged from 60% to 140% at three spiked levels. The detecting indexes in the method cover most forbidden and restricted pesticides,which is meaningful for the safety supervision of the Angelicae Sinensis Radix. With the advantage of rapidness and accuracy,this method can be used for routine determination of multi-pesticides in Angelicae Sinensis Radix.
引文
[1]王莹,金红宇,魏赫,等.花类、果实类中药材中禁限用及常用农药多残留检测方法的建立[J].中国药学杂志,2016(5):404.
[2]王莹,魏赫,乔菲,等.气相色谱-串联质谱法快速筛查人参中192种农药残留[J].中国实验方剂学杂志,2018,24(15):88.
[3]潘孝博,伊雄海,时逸吟,等.液相色谱-高分辨飞行时间质谱法快速筛查食品中香港规例农药残留[J].分析化学,2016(7):1125.
[4]吴姻如,汤旭东,孙超斌,等.基质效应对瓜类蔬菜中有机磷农药残留测定的影响研究[J].农产品质量与安全,2016(4):62.
[5]吕小刚,顾丽莉,孔光辉,等.农药残留前处理及检测的研究进展[J].化工科技,2016(3):86.
[6]贺泽英,刘潇威.农产品中农药残留分析技术研究进展[J].农业资源与环境学报,2016(4):310.
[7]胡磊,李樱红,周明昊.GC测定以植物或真菌为原料的保健食品中有机磷农药残留[J].中国现代应用药学,2017,34(4):563.
[8]刘冰,刘全科,周扬,等. QuEChERS/LC-MS-MS快速测定蔬菜水果中31种氨基甲酸酯类农药残留[J].湖北植保,2016(4):31.
[9]王莹,金红宇,孙磊,等.中药材中198种农药残留测定样品前处理平台的建立[J].药物分析杂志,2011(12):2199.
[10]中国药典.四部[S].2015.
[11]林永强,林林,刘广桢,等.QuEChERS-SPE-UHPLC-MS/MS测定瓜蒌中156种农药残留[J].中国现代应用药学,2018,35(1):17.
[12]佟鹤芳,薛健,吴晓波.中药材农药残留检测方法与标准研究[J].中国现代中药,2011,13(6):49.
[2]王莹,魏赫,乔菲,等.气相色谱-串联质谱法快速筛查人参中192种农药残留[J].中国实验方剂学杂志,2018,24(15):88.
[3]潘孝博,伊雄海,时逸吟,等.液相色谱-高分辨飞行时间质谱法快速筛查食品中香港规例农药残留[J].分析化学,2016(7):1125.
[4]吴姻如,汤旭东,孙超斌,等.基质效应对瓜类蔬菜中有机磷农药残留测定的影响研究[J].农产品质量与安全,2016(4):62.
[5]吕小刚,顾丽莉,孔光辉,等.农药残留前处理及检测的研究进展[J].化工科技,2016(3):86.
[6]贺泽英,刘潇威.农产品中农药残留分析技术研究进展[J].农业资源与环境学报,2016(4):310.
[7]胡磊,李樱红,周明昊.GC测定以植物或真菌为原料的保健食品中有机磷农药残留[J].中国现代应用药学,2017,34(4):563.
[8]刘冰,刘全科,周扬,等. QuEChERS/LC-MS-MS快速测定蔬菜水果中31种氨基甲酸酯类农药残留[J].湖北植保,2016(4):31.
[9]王莹,金红宇,孙磊,等.中药材中198种农药残留测定样品前处理平台的建立[J].药物分析杂志,2011(12):2199.
[10]中国药典.四部[S].2015.
[11]林永强,林林,刘广桢,等.QuEChERS-SPE-UHPLC-MS/MS测定瓜蒌中156种农药残留[J].中国现代应用药学,2018,35(1):17.
[12]佟鹤芳,薛健,吴晓波.中药材农药残留检测方法与标准研究[J].中国现代中药,2011,13(6):49.