固相萃

发布时间：2018-01-14 05:04

本文关键词：固相萃取—加压毛细管电色谱测定水中农药残留　出处：《上海交通大学》2015年硕士论文　论文类型：学位论文

【摘要】：加压毛细管电色谱(pressurized capillary electrochromatography,pCEC)是近年来快速发展的一种高效微分离技术,它兼具高效液相色谱(High Performance Liquid Chromatography,HPLC)和毛细管电泳(Capillary Electrophoresic,CE)的优势,在一台仪器上实现pCEC、CE、微径液相三种分离,具有高柱效、高分离度、高选择性、快速分离、微型化、经济实惠等优点,对复杂化学的分离研究具有重大的意义。本论文主要由四部分组成:第一部分介绍该课题的背景和意义,包括农药种类和水环境污染状况,CEC、pCEC的原理和应用,农药残留分析方法概述等。第二部分建立pCEC-UV分离检测弱极性农药的方法及其在实际水样检测中的应用,该方法以1.8μm C18反相毛细管色谱柱为分离柱,以乙腈-5mM Tris-HCl(pH7.1)(66:34,v/v)为流动相等度洗脱,泵总流速为0.06m L/min,分离电压-9 kV,八种组分可在16min内实现快速分离。线性范围为3.4~100μg/mL(乐果)、8.1~120μg/m L(敌敌畏)、1.2~50μg/mL(克百威)、0.2~50μg/m L(甲萘威)、0.1~50μg/mL(莠去津)、3.7~100μg/mL(甲基对硫磷)、11.2~150μg/m L(马拉硫磷)、2.1~100μg/mL(百菌清);相关系数R为0.9961~0.9997;检测限在0.03~3.7μg/mL之间;加标回收率在71.0~114.1%之间,RSD在1.1~9.8%之间。第三部分建立pCEC-UV分离检测非极性农药的方法及其在实际水样检测中的应用,该方法以乙腈-5mM磷酸缓冲液(pH 6)(90:10,v/v)为流动相等度洗脱,泵总流速0.08m L/min,分离电压为-6 kV,三种组分可在13min内实现快速分离。线性范围为4~100μg/m L(对硫磷)、6~100μg/m L(毒死蜱)、1.5~50μg/mL(溴氰菊酯);相关系数R为0.9966?0.9989;检测限在0.5~2.0μg/m L之间;加标回收率在71.4~107.2%之间,RSD在2.0~9.5%之间。第四部分总结实验的不足和毛细管电色谱未来的展望。
[Abstract]:Pressurized capillary electrochromatography (capillary electrochromatography). PCEC is a highly efficient microseparation technology developed rapidly in recent years. It has high Performance Liquid Chromatography. The advantages of HPLC and Capillary Electrophobic Acid (CEC) have been achieved on a single instrument, which are separated by microdiameter liquid phase. It has the advantages of high column efficiency, high separation degree, high selectivity, rapid separation, miniaturization, economical and so on. This paper mainly consists of four parts: the first part introduces the background and significance of the subject, including pesticide species and water environmental pollution status CEC. The principle and application of pCEC, the summary of pesticide residue analysis methods, etc. In the second part, the method of separation and detection of weakly polar pesticides by pCEC-UV and its application in the detection of real water samples were established. This method was performed on a 1.8 渭 m C18 reversed phase capillary column and a flow equality elution of acetonitrile -5mm Tris-HCln at pH 7.1: 34 v / v). The total flow rate of the pump is 0.06 mL / min, the separation voltage is -9 kV, and the eight components can be separated quickly in 16 minutes. The linear range is 3.4 渭 g / mL (dimethoate). 8.1U 120 渭 g / mL (dichlorvos 1.2g / mL) 50 渭 g / mL (carbaryl 0.2g / mL). 0.1 v 50 渭 g / mL (atrazine 3.7 渭 g / mL) (methyl parathion 11.2v 150 渭 g / mL (malathion). 2.1g / mL, 100 渭 g / mL (Chlorothalonil); The correlation coefficient R was 0.9961U 0.9997; The detection limit was between 0.03 渭 g / mL and 3.7 渭 g / mL. The recoveries were between 71.0% and 114.1%. RSD was between 1.1% and 9.8%. In the third part, a method for the separation and detection of non-polar pesticides by pCEC-UV and its application in the detection of real water samples were established. In this method, acetonitrile-5mm phosphoric acid buffer pH 6: 10: 10 v / v) was used as the flow equal degree of elution, the total pump flow rate was 0.08 mL / min, and the separation voltage was 6 kV. The three components can be separated quickly within 13 minutes. The linear range is 4o 100 渭 g / m L (100 渭 g / m L parathion), and the linear range is 100 渭 g / m L (chlorpyrifos). 1.5 渭 g / mL (deltamethrin); The correlation coefficient R is 0.996 6? 0.9989; The detection limit was between 0.5 渭 g / mL and 2.0 渭 g / mL; The recoveries were between 71.4% and 107.2%, and the RSD was between 2.0 and 9.5%. 4th, the deficiency of the experiment and the prospect of capillary electrochromatography were summarized.
【学位授予单位】：上海交通大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：X839.2;O657.7

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