Solvent-less Analytical Method for Environmental Analysis

本课题的研究结果如下：1)SPMESPME是一种完全不同于现有样品提取方法的基本评价方法，它是一种通过熔融石英毛细管表面涂层（通常是聚合物材料）从基体中提取某些化合物并将这些化合物浓缩在涂层材料中的方法。SPME技术的基本关键是什么样的涂层材料最适合于分析目的，例如，对于环境样品中的农药分析，选择合适的纤维表面涂层，然后利用这种涂层纤维作为工具建立提取条件是重要的。本课题以聚丙烯酸酯涂层为萃取介质，确定了最佳的SPME萃取条件。2)微柱LC（毛细管LC）的基本评价最适合与SPME萃取法相结合的分离方法是微柱LC（毛细管LC）技术，因为这两种技术分别需要非常少量的有机溶剂作为萃取介质和流动相。微柱LC的分离条件与常规柱LC的分离条件不同，因此需要建立水样中农药分析的最佳分离条件。在这个项目中，推荐使用1mm的微柱作为实际样品分析的工具。3) SPME与微柱LC的接口为了实现SPME与微柱LC的接口，需要专门设计的器件。在本工作中，我们研制了该装置，并将其应用于SPME与微柱LC的接口。萃取过程中有机溶剂用量小于30ul。由于微柱LC的典型流动相流速为50 μ min，如果分析时间为60分钟，则需要3 mL溶剂，总溶剂消耗约小于3.1 mL。为了进一步减少消耗，可以使用直径小得多的分离柱，但由于需要完全减少死体积，因此接口装置应该更复杂。4) SPME/微柱LCAs的应用，成功实现了该技术在环境水样农药分析和人尿样品药物分析中的应用。少

In this project the following results were obtained :1)Basic evaluation of SPMESPME which is a totally different from the present sample extraction method, is a method to extract some compounds from the matrix by the surface coating (usually polymeric material) on fused-silica capillary and concentrate those compounds in the coating material. The basic key point in SPME technique is what kind of coating materials will be the most suitable for the analytical purposes, for example, for pesticides analysis in environmental samples, choosing the appropriate coating of the fiber surface and then using such coating fiber as a tool to establish the extraction conditions are the important. In this project the best SPME conditions were established by using polyacryrate coating as the extraction medium.2) Basic evaluation of microcolumn LC (Capillary LC)The scparation method which is most suitable to combine to SPME extraction method is the technique so-called microcolumn LC(Capillary LC), becau … More se both techniques do require very small amount of organic solvents as the extraction medium and the mobile phase, respectively. For microcolumn LC the separation conditions should be different from that with conventional column LC and therefore we have needed to establish the best separation conditions for pesticides analysis in water samples. In this project 1 mm i.d. microcolumn was recommended as the tool for actual sample analysis.3) Interfacing between SPME and microcolumn LCIn order to interface SPME to microcolumn LC,the device specially designed is required. In this work we have developed the device and applied it to the interfacing between SPME and microcolumn LC.The required amount of organic solvents for the extraction process is less than 30 uL.Since the typical mobile phase flow rate is 50 uLomin for microcolumn LC,if the analysis time is 60 minutes, 3 mL solvent is required and total solvents consumption is about less than 3.1 mL.To reduce the consumption more, one can use much smaller diameter columns for the separation but the interfectly device should be more complicated because the dead volume should be perfectly reduced.4) Application of SPME/microcolumn LCAs the application of this technique pesticides analysis in environmental water samples and drug analysis in human urine samples were successfully performed. Less