作者：张伟¹, 陈静¹, 文凤伟², 李明明¹

作者单位：1. 山东省临沂生态环境监测中心，山东 临沂 276000;
2. 临沂市生态环境综合执法支队兰山大队， 山东 临沂 276000

关键词：加压液体提取;自动固相萃取;液相色谱-质谱联用仪;吡啶类农药

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0.001~5.0 μg/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、0.005 μg/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。

Determination of six pyridine pesticide residues in agricultural soil by pressurized liquid extraction-automatic SPE-UPLC-MS/MS method
ZHANG Wei¹, CHEN Jing¹, WEN Fengwei², LI Mingming¹
1. Shandong Linyi Ecological Environment Monitoring Center, Linyi 276000, China;
2. Lanshan Brigade of Linyi Ecological Environment Comprehensive Law Enforcement Detachment, Linyi 276000, China
Abstract: 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 column was put into automatic solid phase extraction instrument. After activation, the program was set, the above extraction solution was passed through the solid phase extraction column at a flow rate of 20 mL/min, and finally eluted with 20 mL methanol-acetonitrile (V∶V =1∶1). The eluent was collected and blown to nearly dry by nitrogen. The residue was dissolved by 1 mL methanol and volexed, then qualitatively and quantitatively detected on UPLC-MS/MS. Picoxystrobin, fluridone, imidacloprid, boscalid, fluopicolide and acetamiprid showed good linear relationships in the concentration ranges of 0.001 to 5.0 μg/mL, with correlation coefficients 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 standard deviation(RSD) of repeatability(n=6) were 2.0%, 3.1%, 2.3%, 2.2%, 1.9% and 2.3%. The experimental results showed that the method was accurate, sensitive and suitable for the determination of trace pyridine pesticide residues in agricultural soil.
Keywords: pressurized liquid extraction;automatic SPE;HPLC-MS/MS;pyridine pesticides
2024, 50(4):68-73  收稿日期: 2022-02-17;收到修改稿日期: 2022-04-19
基金项目:
作者简介: 张伟(1982-),女,山东兰陵县人,高级工程师,硕士,主要从事环境监测工作。
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