本文關鍵詞：固相萃取—加壓毛細管電色譜測定水中農藥殘留　出處：《上海交通大學》2015年碩士論文　論文類型：學位論文

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【摘要】：加壓毛細管電色譜(pressurized capillary electrochromatography,pCEC)是近年來快速發(fā)展的一種高效微分離技術,它兼具高效液相色譜(High Performance Liquid Chromatography,HPLC)和毛細管電泳(Capillary Electrophoresic,CE)的優(yōu)勢,在一臺儀器上實現(xiàn)pCEC、CE、微徑液相三種分離,具有高柱效、高分離度、高選擇性、快速分離、微型化、經濟實惠等優(yōu)點,對復雜化學的分離研究具有重大的意義。本論文主要由四部分組成:第一部分介紹該課題的背景和意義,包括農藥種類和水環(huán)境污染狀況,CEC、pCEC的原理和應用,農藥殘留分析方法概述等。第二部分建立pCEC-UV分離檢測弱極性農藥的方法及其在實際水樣檢測中的應用,該方法以1.8μm C18反相毛細管色譜柱為分離柱,以乙腈-5mM Tris-HCl(pH7.1)(66:34,v/v)為流動相等度洗脫,泵總流速為0.06m L/min,分離電壓-9 kV,八種組分可在16min內實現(xiàn)快速分離。線性范圍為3.4~100μg/mL(樂果)、8.1~120μg/m L(敵敵畏)、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(甲基對硫磷)、11.2~150μg/m L(馬拉硫磷)、2.1~100μg/mL(百菌清);相關系數(shù)R為0.9961~0.9997;檢測限在0.03~3.7μg/mL之間;加標回收率在71.0~114.1%之間,RSD在1.1~9.8%之間。第三部分建立pCEC-UV分離檢測非極性農藥的方法及其在實際水樣檢測中的應用,該方法以乙腈-5mM磷酸緩沖液(pH 6)(90:10,v/v)為流動相等度洗脫,泵總流速0.08m L/min,分離電壓為-6 kV,三種組分可在13min內實現(xiàn)快速分離。線性范圍為4~100μg/m L(對硫磷)、6~100μg/m L(毒死蜱)、1.5~50μg/mL(溴氰菊酯);相關系數(shù)R為0.9966?0.9989;檢測限在0.5~2.0μg/m L之間;加標回收率在71.4~107.2%之間,RSD在2.0~9.5%之間。第四部分總結實驗的不足和毛細管電色譜未來的展望。
[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.
【學位授予單位】：上海交通大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：X839.2;O657.7

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本文編號：1422114