分散固相萃取-液质联用法测定稻渔综合种养环境中四种农药残留
Determination of four pesticide residues in rice-aquaculture integrated cultivation environment using dispersion solid phase extraction-high performance liquid chromatography-tandem mass spectromentry method
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摘要: 建立了液相色谱-串联质谱法（HPLC-MS/MS）同时测定稻渔综合种养环境中苄嘧磺隆、双草醚、吡蚜酮和氯虫苯甲酰胺的分析方法.水样过滤后直接进样，土壤和水产品经乙腈匀浆提取，C18吸附剂净化.结果表明，在不同基质中，4种农药在各自的线性范围内线性关系良好（R2 ≥0.995）；水中氯虫苯甲酰胺的检出限为0.10 μg·kg-1，其它3种为0.05 μg·kg-1；土壤和水产品中氯虫苯甲酰胺的检出限（LOD）为0.20 μg·kg-1，其它3种为0.10 μg·kg-1；在不同添加水平下，4种农药的平均回收率为77.52%—93.86%，相对标准偏差（RSD）为3.73%—11.09%.Abstract: A method was developed for the simultaneous determination of bensulfuron methyl, bispyribac-sodium, pymetrozine and chlorantraniliprole in rice-aquaculture integrated cultivation environment by high performance liquid chromatography-tandem mass spectrometry. Water samples were analyzed directly after filtration. Soil and aquatic products were extracted with acetonitrile and purified by C18 adsorbents. The results showed that good linearity was obtained for the four pesticides in their respective linear ranges, and the correlation coefficients were above 0.995. In water, the limit of detection (LOD) of chlorantraniliprole was found to be 0.10 μg·kg-1, while the other three pesticides were 0.05 μg·kg-1. In soil and aquatic products, the LOD of chlorantraniliprole was 0.20 μg·kg-1, and the other three were 0.10 μg·kg-1. The mean spiked recoveries of four pesticides at different spiked levels ranged from 77.52% to 93.86% with the relative standard deviations (RSDs) of 3.73%-11.09%.
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