摘要
以农业土壤为研究对象,建立采用加压液体提取法将样品中啶氧菌酯、氟啶草酮、吡虫啉、啶酰菌胺、氟啶酰菌胺、啶虫脒6种吡啶类农药提取出来,全自动固相萃取法富集、净化,超高效液相色谱-质谱联用仪定量检测的分析方法。取农业土壤样品,风干、粉碎后,过120目筛,准确称取过筛网后的样品10 g,置萃取池中,加硅藻土20 g,用甲醇:丙酮溶剂(V∶V=1∶1)提取,另取规格为500 mg/12 mL HLB固相萃取小柱,置全自动固相萃取仪中,活化完毕后,设定程序,将上述提取液以20 mL/min的流量,过固相萃取柱,最后用20 mL甲醇-乙腈(V∶V=1∶1)洗脱,收集洗脱液,洗脱液氮吹至近干,加甲醇定容至1 mL,涡旋混匀,上液相色谱-质谱仪定性、定量检测。啶氧菌酯、氟啶草酮、吡虫啉、啶酰菌胺、氟啶酰菌胺、啶虫脒6种吡啶类农药在0.001~5.0μg/mL范围内具有良好的线性,相关系数均大于0.995;检测限分别为0.012、0.009、0.024、0.007、0.013、0.005μg/L。三水平加标回收率均在84.4%~105.2%之间;重复性RSD(n=6)分别为2.0%、3.1%、2.3%、2.2%、1.9%和2.3%。实验结果表明,实验建立的方法具有准确、灵敏等优点,适用于农业土壤中微量吡啶类农药残留的检测。
A pressurized liquid extraction method was established to extract six pyridine pesticides from the samples,including picoxystrobin,fluridone,imidacloprid,boscalid,fluopicolide,and acetamiprid.The method,takes agricultural soil as the research object,which was enriched and purified by automatic solid phase extraction,and quantitated by ultra-performance liquid chromatography-mass spectrometry(UPLC-MS/MS).Agricultural soil samples were taken,dried and crushed,and passed through a 120-mesh sieve.10 g of the screened sample was accurately weighed to the extraction tank,20 g diatomite was added,methanol and acetone solvent (V∶V=1∶1) was selected as extract solution. 500 mg/12 mL HLB solid phase extraction columnwas put into automatic solid phase extraction instrument. After activation, the program was set, the aboveextraction solution was passed through the solid phase extraction column at a flow rate of 20 mL/min, andfinally eluted with 20 mL methanol-acetonitrile (V∶V =1∶1). The eluent was collected and blown to nearly dryby nitrogen. The residue was dissolved by 1 mL methanol and volexed, then qualitatively and quantitativelydetected on UPLC-MS/MS. Picoxystrobin, fluridone, imidacloprid, boscalid, fluopicolide and acetamipridshowed good linear relationships in the concentration ranges of 0.001 to 5.0 μg/mL, with correlationcoefficients all greater than 0.995. Detection limits were 0.012, 0.009, 0.024, 0.007, 0.013, 0.005 μg/L,respectively. Average recoveries in 3 concentration levels were 84.4%-105.2%. Relative standarddeviation(RSD) of repeatability(n=6) were 2.0%, 3.1%, 2.3%, 2.2%, 1.9% and 2.3%. The experimental resultsshowed that the method was accurate, sensitive and suitable for the determination of trace pyridine pesticideresidues in agricultural soil.
作者
张伟
陈静
文凤伟
李明明
ZHANG Wei;CHEN Jing;WEN Fengwei;LI Mingming(Shandong Linyi Ecological Environment Monitoring Center,Linyi 276000,China;Lanshan Brigade of Linyi Ecological Environment Comprehensive Law Enforcement Detachment,Linyi 276000,China)
出处
《中国测试》
CAS
北大核心
2024年第4期68-73,共6页
China Measurement & Test
