作者：尹平艳, 何玉霜, 杨华, 段绍恒, 陈煦, 凌慧娇

作者单位：广西壮族自治区环境保护科学研究院，广西 南宁 530022

关键词：加速溶剂萃取;河道淤泥;UPLC-MS/MS;氨基甲酸酯类;农药

摘要：

建立ASE法提取耕地周边河道淤泥中的XMC、猛杀威、恶虫威、仲丁威、灭多威、残杀威和脱甲基抗蚜威UPLC-MS/MS法定性、定量检测的分析方法。随机采集耕地周边河道淤泥样品，风干、粉碎、过筛后，准确称取约8 g样品，置全自动加速溶剂萃取仪中提取。提取液经凝胶净化色谱净化，净化液氮吹至近干，加1 mL甲醇溶解，0.45 μm滤膜过滤后，上UPLC-MS/MS仪定性、定量检测。XMC、猛杀威、恶虫威、仲丁威、灭多威、残杀威和脱甲基抗蚜威在0.02~5.0 μg/mL浓度范围内具有良好的线性；检出限分别为0.082 μg/kg、0.051 μg/kg、0.173 μg/kg、0.147 μg/kg、0.054 μg/kg、0.084 μg/kg和0.035 μg/kg；平均加样回收率在86.9%~105.9%之间；重复性RSD（n=6）测试结果均在5.0%以内。结果表明，此方法具有检测准确度高、重复性好、检出限低等优点，适用于耕地河道淤泥中氨基甲酸酯类农药残留的检测，为本地耕地种植农药的合理使用提供技术参考。

Determination of seven carbamate pesticide residues in river sludge around cultivated land by UPLC-MS/MS
YIN Pingyan, HE Yushuang, YANG Hua, DUAN Shaoheng, CHEN Xu, LING Huijiao
Guangxi Zhuang Autonomous Region Academy of Environmental Protection, Nanning 530022, China
Abstract: An analytical method was established for qualitative and quantitative analysis of XMC, promecarb, bendiocarb, fenobucarb, methomyl, propoxur and pirimicarb in river silt around cultivated land by automatic solid phase extraction(ASE)-UPLC-MS/MS. Samples of river silt were randomly collected. After drying, crushing and sieving, about 8 g samples was accurately weighed to ASE for extraction. The extract was purified by gel purification and chromatography(GPC). Purified liquid was blown to near dry by nitrogen and 1 mL methanol was added for dissolution. After 0.45 μm membrane filtration, UPLC-MS /MS was used for qualitative and quantitative detection. XMC, promecarb, bendiocarb, fenobucarb, methomyl, propoxur and pirimicarb showed good linear relationships in the concentration range 0.02-5.0 μg/mL. The detection limits were 0.082 μg/kg, 0.051 μg/kg, 0.173 μg/kg, 0.147 μg/kg, 0.054 μg/kg, 0.084 μg/kg and 0.035 μg/kg, respectively. Average recoveries were ranged from 86.9%-105.9%. Relative standard deviation(RSD) of repeatability was below 5% (n=6). Conclusion The results showed that this method has the advantages of high accuracy, good repeatability and low detection limit, which is suitable for the detection of carbamate pesticide residues in river silt of cultivated land. It also provides a technical reference for the rational use of pesticides in local cultivated land.
Keywords: ASE;river silt;UPLC-MS/MS;carbamates;pesticides
2022, 48(7):77-82  收稿日期: 2021-08-09;收到修改稿日期: 2021-09-28
基金项目:
作者简介: 尹平艳（1987-），女，广西南宁市人，工程师，从事环境保护和环境监测工作
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