Vílchez J L, Prieto A, Araujo L, Navalón A
Department of Analytical Chemistry, University of Granada, Spain.
J Chromatogr A. 2001 Jun 1;919(1):215-21. doi: 10.1016/s0021-9673(01)00788-9.
A method for the determination of trace amounts of the insecticide fipronil was developed using solid-phase microextraction-gas chromatography-mass spectrometry and selected ion monitoring. Fipronil was extracted with a fused-silica fiber coated with 85 microm polyacrylate. The effects of pH, ionic strength, sample volume, extraction and desorption times as well as the extraction temperature were studied. Lindane was used as an internal standard. The linear concentration range of application was 0.3-100 ng ml(-1) of fipronil, with a relative standard deviation of 9.5% (for a level of 50 ng ml(-1)) and a detection limit of 0.08 ng ml(-1). The method was applied to check the eventual existence of fipronil above this limit in water and soil samples from Granada (Spain) as well as in human urine samples. The method validation was completed with spiked matrix samples. The method can be applied as a monitoring tool for water, soil and urine, in the investigation of environmental and occupational exposure to fipronil.
建立了一种采用固相微萃取-气相色谱-质谱联用及选择离子监测法测定痕量杀虫剂氟虫腈的方法。用涂有85微米聚丙烯酸酯的熔融石英纤维萃取氟虫腈。研究了pH值、离子强度、样品体积、萃取和解吸时间以及萃取温度的影响。以林丹为内标。氟虫腈的线性应用浓度范围为0.3-100 ng ml⁻¹，相对标准偏差为9.5%（对于50 ng ml⁻¹的水平），检测限为0.08 ng ml⁻¹。该方法用于检测西班牙格拉纳达的水、土壤样品以及人体尿液样品中是否存在高于此限度的氟虫腈。通过加标基质样品完成了方法验证。该方法可作为水、土壤和尿液的监测工具，用于调查环境和职业性氟虫腈暴露情况。
