Ma Jiping, Lu Xi, Xia Yan, Yan Fengli
Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China
Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China.
J Chromatogr Sci. 2015 Feb;53(2):380-4. doi: 10.1093/chromsci/bmu055. Epub 2014 Jun 19.
A solid-phase extraction (SPE) method using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography was developed for the determination of four pyrazole and pyrrole pesticides (fenpyroximate, chlorfenapyr, fipronil and flusilazole) in environmental water samples. Several parameters, such as extraction adsorbent, elution solvent and volume and sample loading flow rate were optimized to obtain high SPE recoveries and extraction efficiency. The calibration curves for the pesticides extracted were linear in the range of 0.05-10 μg L(-1) for chlorfenapyr and fenpyroximate and 0.05-20 μg L(-1) for fipronil and flusilazole, with the correlation coefficients (r(2)) between 0.9966 and 0.9990. The method gave good precisions (relative standard deviation %) from 2.9 to 10.1% for real spiked samples from reservoir water and seawater; method recoveries ranged 92.2-105.9 and 98.5-103.9% for real spiked samples from reservoir water and seawater, respectively. Limits of detection (S/N = 3) for the method were determined to be 8-19 ng L(-1). The optimized method was successfully applied to the determination of four pesticides of pyrazoles and pyrroles in real environmental water samples.
建立了一种以多壁碳纳米管为吸附剂的固相萃取（SPE）方法，并与高效液相色谱联用，用于测定环境水样中的四种吡唑和吡咯类农药（唑螨酯、虫螨腈、氟虫腈和氟硅唑）。对萃取吸附剂、洗脱溶剂及体积、进样流速等参数进行了优化，以获得较高的固相萃取回收率和萃取效率。所萃取农药的校准曲线在0.05 - 10 μg L⁻¹（唑螨酯和虫螨腈）以及0.05 - 20 μg L⁻¹（氟虫腈和氟硅唑）范围内呈线性，相关系数（r²）在0.9966至0.9990之间。对于来自水库水和海水的实际加标样品，该方法具有良好的精密度（相对标准偏差%），范围为2.9%至10.1%；来自水库水和海水的实际加标样品的方法回收率分别为92.2 - 105.9%和98.5 - 103.9%。该方法的检测限（S/N = 3）确定为8 - 19 ng L⁻¹。该优化方法成功应用于实际环境水样中四种吡唑和吡咯类农药的测定。
