QuEChERS-高效液相色谱-串联四极杆飞行时间质谱法同时测定大米中7种除草剂残留
投稿时间:2019-02-01      点此下载全文 HTML
引用本文:徐江艳,施瑛,高贝贝,等.QuEChERS-高效液相色谱-串联四极杆飞行时间质谱法同时测定大米中7种除草剂残留[J].农药学学报,2019,21(4):468-474.
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作者单位E-mail
徐江艳 南京农业大学 理学院, 南京 210095  
施瑛 南京农业大学 理学院, 南京 210095  
高贝贝 南京农业大学 植物保护学院, 南京 210095  
张召贤 南京农业大学 植物保护学院, 南京 210095  
温勇 南京农业大学 植物保护学院, 南京 210095  
吕波 南京农业大学 理学院, 南京 210095 njndlb@njau.edu.cn 
基金项目:中央高校基本科研业务费资助项目(Y0201700423);国家重点研发计划项目(2018YFD0200503)
中文摘要:建立了同时测定大米中西草净、异丙隆、苄嘧磺隆、莎稗磷、乙氧氟草醚、噁草酮和二甲戊灵7种除草剂残留的QuEChERS-高效液相色谱-串联四极杆飞行时间质谱(HPLC-MS/MS Triple TOF)方法。样品经V(乙酸乙酯):V(水)= 80:20混合溶液提取,以N-丙基乙二胺(PSA)为吸附剂进行基质分散萃取净化,采用HPLC-MS/MS Triple TOF检测,外标法定量。结果表明:7种除草剂在一定的质量浓度范围内,其峰面积与对应的质量浓度间线性关系良好,相关系数均大于0.99;西草净、异丙隆、苄嘧磺隆和莎稗磷在0.001、0.01、0.05 mg/kg 3个添加水平下的平均回收率在75%~108%之间,相对标准偏差(RSD)在1.1%~7.0%(n = 5)之间,定量限(LOQ)均为0.001 mg/kg;乙氧氟草醚、噁草酮和二甲戊灵在0.01、0.05和1 mg/kg 3个添加水平下的平均回收率在81%~108%之间,RSD在2.7%~9.0%之间,LOQ均为0.01 mg/kg。该方法样品前处理简单快速,方法灵敏度、准确度和精密度均符合农药残留检测要求,可用于大米中西草净、异丙隆、苄嘧磺隆、莎稗磷、乙氧氟草醚、噁草酮和二甲戊灵残留的同时检测。
中文关键词:QuEChERS  高效液相色谱-串联四极杆飞行时间质谱  大米  除草剂  残留
 
Simultaneous determination of seven herbicide residues in rice using QuEChERS-high performance liquid chromatography-tandem mass spectrometry Triple TOF
Abstract:A multi-residue method was established to simultaneously determine seven herbicides (simetryn, isoproturon, bensulfuron methyl, anilofos, oxyfluorfen, oxadiazon and pendimethalin) in rice using QuEChERS and high performance liquid chromatography-tandem mass spectrometry Triple TOF (HPLC-MS/MS Triple TOF). The samples were extracted with a mixture of ethyl acetate and water (Vethyl acetate:Vwater=80:20), purified by dispersive solid phase extraction with primary secondary amine (PSA), and detected by HPLC-MS/MS Triple TOF using the external standard method for quantitative analysis. Good linearity was achieved with a correlation coefficient of 0.99. The average recoveries of simetryn, isoproturon, bensulfuron methyl and anilofos ranged from 75% to 108% with the spiked levels of 0.001, 0.01 and 0.05 mg/kg. And the relative standard deviation (RSD) ranged from 1.1% to 7.0% (n=5). The limits of quantification (LOQs) of all those herbicides were 0.001 mg/kg. The average recoveries of oxyfluorfen, oxadiazon and pendimethalin ranged from 81% to 108% with the spiked levels of 0.01, 0.05 and 1 mg/kg. And the RSD ranged from 2.9% to 9.0% (n=5). And their LOQs were 0.01 mg/kg. This method is simple and rapid. Its sensitivity, accuracy and precision can meet the requirements of the pesticide residue analysis. Therefore, this method can be applied to the simultaneous analysis of simetryn, isoproturon, bensulfuron methyl, anilofos, oxyfluorfen, oxadiazon and pendimethalin in rice.
Key words:QuEChERS  high performance liquid chromatography-tandem mass spectrometry Triple TOF (HPLC-MS/MS Triple TOF)  rice  herbicide  residue
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