比较两种离子液体分散液液微萃取方法，用于使用液相色谱-四极杆线性离子阱质谱法测定废水中的苯甲酰脲类杀虫剂：绿色参数评估。
Comparison of two ionic liquid dispersive liquid-liquid microextraction approaches for the determination of benzoylurea insecticides in wastewater using liquid chromatography-quadrupole-linear ion trap-mass spectrometry: evaluation of green parameters.
机构信息
Department of Chemistry and Physics, University of Almería, Centro de Investigación en Biotecnología Agroalimentaria, Area of Analytical Chemistry, BITAL, Campus de Excelencia Agroalimentario, ceiA3, La Cañada de San Urbano, E-04120 Almería, Spain.
Department of Chemistry and Physics, University of Almería, Centro de Investigación en Biotecnología Agroalimentaria, Area of Analytical Chemistry, BITAL, Campus de Excelencia Agroalimentario, ceiA3, La Cañada de San Urbano, E-04120 Almería, Spain.
出版信息
J Chromatogr A. 2014 Aug 22;1356:1-9. doi: 10.1016/j.chroma.2014.06.032. Epub 2014 Jun 18.
Two dispersive liquid-liquid microextraction (DLLME) approaches including temperature-controlled ionic liquid dispersive liquid-liquid microextraction (TCIL-DLLME) and ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) were compared for the extraction of six benzoylurea insecticides (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, lufenuron and flufenoxuron) from wastewater samples prior to their determination by high-performance liquid chromatography with a hybrid triple quadrupole-linear ion trap-mass spectrometer (LC-QqLIT-MS/MS). Influential parameters affecting extraction efficiency were systematically studied and optimized and the most significant green parameters were quantified and compared. The best results were obtained using the US-IL-DLLME procedure, which employed the IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C8MIM][PF6]) and methanol (MeOH) as extraction and disperser solvent, respectively. US-IL-DLLME procedure was fast, easy, low environmental toxicity and, it was also able to successfully extract all selected benzoylureas. This method was extensively validated with satisfactory results: limits of detection and quantification were in the range 0.5-1.0 ng L(-1) and 1.5-3.5 ng L(-1), respectively, whereas recovery rates ranged from 89 to 103% and the relative standard deviations were lower than 13.4%. The applicability of the method was assessed with the analysis of effluent wastewater samples from a wastewater treatment plant located in an agricultural zone of Almería (Spain) and the results indicated the presence of teflubenzuron at mean concentration levels of 11.3 ng L(-1). US-IL-DLLME sample treatment in combination with LC-QqLIT-MS/MS has demonstrated to be a sensitive, selective and efficient method to determine benzoylurea insecticides in wastewaters at ultra-trace levels.
两种分散液液微萃取（DLLME）方法，包括温度控制离子液体分散液液微萃取（TCIL-DLLME）和超声辅助离子液体分散液液微萃取（US-IL-DLLME），被用于从废水样品中萃取六种苯甲酰脲类杀虫剂（除虫脲、伏虫隆、氟铃脲、噻虫隆、氟虫脲和虱螨脲），然后用高效液相色谱-混合三重四极杆-线性离子阱-质谱联用仪（LC-QqLIT-MS/MS）进行测定。系统研究并优化了影响萃取效率的影响因素，并对最显著的绿色参数进行了量化和比较。采用 US-IL-DLLME 法，使用 IL 1-辛基-3-甲基咪唑六氟磷酸盐（[C8MIM][PF6]）和甲醇（MeOH）分别作为萃取和分散溶剂，获得了最佳结果。US-IL-DLLME 法快速、简单、环境毒性低，并且能够成功萃取所有选定的苯甲酰脲类杀虫剂。该方法经过广泛验证，结果令人满意：检出限和定量限分别在 0.5-1.0 ng L(-1)和 1.5-3.5 ng L(-1)范围内，回收率在 89-103%之间，相对标准偏差低于 13.4%。该方法的适用性通过分析位于阿尔梅里亚（西班牙）农业区的一家污水处理厂的废水进行了评估，结果表明在废水中存在氟铃脲，其平均浓度水平为 11.3 ng L(-1)。结合 LC-QqLIT-MS/MS 的 US-IL-DLLME 样品处理方法，已被证明是一种用于测定废水中痕量苯甲酰脲类杀虫剂的灵敏、选择性和高效方法。
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