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对用膜萃取和流动注射技术进行样品的在线预处理方法进行了较为系统的研究。第一部分提出了一种新的样品前处理技术———连续流动液膜萃取(CFLME),并用于极性有机污染物的痕量富集。阐述了CFLME的基本原理,并以磺酰脲类除草剂和内分泌干扰物双酚 A为模型化合物,研究了CFLME的影响因素。在优化的条件下,甲磺隆和双酚 A分别经过 1 2 0min和 40min的萃取后,可达到 1 0 0 0倍和2 0 0倍的富集倍数,富集效率是SLM的 3.5～ 2 0 0倍。在此基础上,建立了CFLME 高效液相色谱(HPLC)在线联用测定磺酰脲类除草剂的方法,样品富集 1 0min就能达到 0.0 5～ 0.1 μg/L的检测限;建立的CFLME C1 8预柱 HPLC/紫外检测器在线联用系统,可测定地表水中ng/L级的磺酰脲类除草剂,其检测限比用C1 8SPE柱富集、HPLC/紫外检测器测定时低 2 0 0倍。研究表明,CFLME的主要优点是高选择性、高富集效率、低成本、液膜长期稳定,并易与各种分析仪器联用。第二部分研究了几种流动注射(FI)在线样品前处理技术,为FI应用于日常分析提供了新的思路和途径。建立了FI微孔膜液萃取(MM LLE)系统,用于洗涤剂中阴离子表面活性剂的日常测定;发展了FI高温反应系统,并成功地用于洗涤剂中的总无机磷酸盐以及烟草中总还原糖的自动分析;提出用试剂注入 FI技术
A systematic study of online pretreatment of samples using membrane extraction and flow injection techniques was carried out. In the first part, a new sample preparation technique, CFLME, is proposed and used for the trace enrichment of polar organic pollutants. The basic principle of CFLME was expounded, and the influencing factors of CFLME were studied by using sulfonylurea herbicide and bisphenol A, an endocrine disruptor. Under the optimal conditions, the extraction efficiency of metsulfuron and bisphenol A reached 100% and 200% after 120 min and 40 min respectively, and the enrichment efficiency was 3.5 ~ 2 0 0 times. On this basis, a method for on-line determination of sulfonylurea herbicides by CFLME high performance liquid chromatography (HPLC) was established. The detection limit of 0.0 5 ~ 0.1 μg / L could be reached after the sample was concentrated for 10 min. The established CFLME C1 8 pre-column HPLC / UV detector online system, can be measured surface water ng / L sulfonylurea herbicides, the detection limit than the C1 8SPE column enrichment, HPLC / UV detector measured low 2 0 0 times. The research shows that the main advantages of CFLME are high selectivity, high enrichment efficiency, low cost, long-term stability of the liquid film and ease of use with various analytical instruments. In the second part, several flow injection (FI) on-line sample preparation techniques are studied, providing new ideas and approaches for the FI application in routine analysis. The FI Micropore Membrane Fluid Extraction (MM LLE) system was established for the routine determination of anionic surfactants in detergents; the FI high temperature reaction system was developed and successfully used in total inorganic phosphate in detergents as well as in tobacco Automatic analysis of total reducing sugars; proposed injection of FI technology with reagents