State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
Anal Chim Acta. 2015 Feb 20;860:29-36. doi: 10.1016/j.aca.2014.12.047. Epub 2014 Dec 30.
In present study, a convenient, sensitive and environmentally friendly method for the determination of five benzoylurea insecticides (BUs) in water and juice samples was developed. To extract trace benzoylurea insecticides effectively, poly(methacrylic acid-co-ethylene dimethacrylate) monolith was prepared and used as the sorbent of multiple monolithic fiber solid-phase microextraction (MMF-SPME). The influences of preparation conditions of monolith and extraction parameters of MMF-SPME on BUs were studied thoroughly. Under the optimized conditions, the combination of MMF-SPME with high performance liquid chromatography-diode array detection (MMF-SPME-HPLC-DAD) showed expected analytical performance for target analytes. The limits of detection (S/N=3) of the developed method were 0.026-0.075 μg L(-1) in water and 0.053-0.29 μg L(-1) in juice samples. Good linearity was obtained for analytes with the correlation coefficients (R(2)) above 0.99. Satisfactory repeatability and reproducibility was achieved, with relative standard deviations (RSD) of both less than 10%. Finally, the established MMF-SPME-HPLC-DAD method was successfully applied for the determination of BUs residues in juice and environmental water samples. Recoveries obtained for the determination of BUs in spiking samples ranged from 65.1% to 118%, with RSD below 10% in all cases.
在本研究中,开发了一种用于水样和果汁样品中五种苯甲酰脲类杀虫剂(BUs)测定的简便、灵敏、环保的方法。为了有效提取痕量苯甲酰脲类杀虫剂,制备了聚(甲基丙烯酸-co-乙二醇二甲基丙烯酸酯)整体柱,并将其用作多根整体纤维固相微萃取(MMF-SPME)的吸附剂。详细研究了整体柱的制备条件和 MMF-SPME 的萃取参数对 BUs 的影响。在优化条件下,MMF-SPME 与高效液相色谱-二极管阵列检测(MMF-SPME-HPLC-DAD)的组合对目标分析物表现出预期的分析性能。该方法的检出限(S/N=3)在水样中为 0.026-0.075μg/L,在果汁样品中为 0.053-0.29μg/L。分析物的线性相关性良好,相关系数(R²)均大于 0.99。得到了令人满意的重复性和重现性,相对标准偏差(RSD)均小于 10%。最后,建立的 MMF-SPME-HPLC-DAD 方法成功应用于果汁和环境水样中 BUs 残留的测定。在加标样品的测定中,BUs 的回收率在 65.1%至 118%之间,所有情况下的 RSD 均低于 10%。