摘要
[目的]基于经典的QuEChERS前处理方法,结合高效液相色谱串联质谱(HPLC-MS/MS)建立四唑虫酰胺在马铃薯及土壤中残留分析方法,明确四唑虫酰胺在马铃薯和土壤中的消解行为和最终残留。[方法]样品经乙腈提取,50 mg PSA、20 mg GCB和100 mg无水MgSO4净化,以5 mmol/L乙酸铵水溶液-乙腈为流动相进行梯度洗脱,HPLC-MS/MS测定,外标法定量。[结果]四唑虫酰胺在马铃薯块茎、马铃薯植株和土壤中0.001~1.0 mg/L质量浓度范围内色谱峰面积与质量浓度呈现良好线性(r>0.9995);在添加水平0.01~15 mg/kg下,3种基质中的四唑虫酰胺平均回收率均处于84.1%~108.1%之间,相对标准偏差(RSD)均处于1.1%~8.4%之间。四唑虫酰胺的定量限(LOQ)为0.01 mg/kg。四唑虫酰胺在马铃薯块茎、马铃薯植株和土壤中的消解动态符合一级动力学方程,半衰期分别为3.8~9.4、3.9~4.0、11.8~28.1 d,四唑虫酰胺在马铃薯块茎和土壤中的最终残留量为<0.01 mg/kg,在马铃薯植株中的最终残留量为<0.01~1.495 mg/kg。[结论]该方法简单、快速、可靠,符合农药残留分析要求,适用于马铃薯中四唑虫酰胺残留量的检测。试验可为四唑虫酰胺在马铃薯上的安全合理施用提供数据支持。
[Aims]Based on QuEChERS pretreatment and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),a method for the determination of tetraniliprole residues in potatoes and soil was established,to clarify the dissipation behavior and final residue of tetraniliprole.[Methods]The samples were extracted by acetonitrile,cleaned-up by a mixture of PSA(50 mg),GCB(20 mg)and anhydrous MgSO4(100 mg),and eluted by gradient elution with 5 mmol/L aqueous ammonium acetate-acetonitrile as the mobile phase,and then determined by HPLC-MS/MS and quantified by the external standard method.[Results]The chromatographic peak areas of tetraniliprole in potato tuber,potato plant and soil samples showed good linearity(r>0.9995)with the mass concentration in the range of 0.001-1.0 mg/L.The average recoveries of tetraniliprole in the 3 matrices at the spiked levels of 0.01-15 mg/kg ranged from 84.1%to 108.1%,with the relative standard deviations(RSDs)of 1.1%-8.4%.The limit of quantification(LOQ)of tetraniliprole was 0.01 mg/kg.The dissipation dynamics of tetraniliprole in potato tuber,potato plant and soil samples conformed to the first-order kinetic equation with the half-lives of 3.8-9.4,3.9-4.0 and 11.8-28.1 d,respectively.The final residue of tetraniliprole was<0.01 mg/kg in potato tuber and soil,and<0.01-1.495 mg/kg in potato plant.[Conclusions]The method is simple,rapid,reliable and suitable for the determination of tetraniliprole residues in potatoes.This study can provide a supporting data for safe and rational application of tetraniliprole on potatoes.
作者
汪庆屹
赵庆慧
程志加
张宁
王雅贺
宋明霞
郭金博
吕佳旭
刘洋
侯志广
逯忠斌
WANG Qingyi;ZHAO Qinghui;CHENG Zhijia;ZHANG Ning;WANG Yahe;SONG Mingxia;GUO Jinbo;LYU Jiaxu;LIU Yang;HOU Zhiguang;LU Zhongbin(College of Plant Protection,Jilin Agricultural University,Changchun 130118,China)
出处
《农药》
CAS
CSCD
北大核心
2024年第6期412-418,共7页
Agrochemicals
基金
农业部行业标准制定嘧菌环胺在人参中的残留限量标准(14202008)。
