岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2014年
3期
406-412
,共7页
地下水%拟除虫菊酯%有机氯农药%百菌清%毒死蜱%气相色谱法%液液萃取
地下水%擬除蟲菊酯%有機氯農藥%百菌清%毒死蜱%氣相色譜法%液液萃取
지하수%의제충국지%유궤록농약%백균청%독사비%기상색보법%액액췌취
underground water%pyrethroids%organochlorine pesticides%chlorothalonil%chlorpyrifos%Gas Chromatography%liquid-liquid extraction
拟除虫菊酯类、有机氯、百菌清等农药均属于电负性强化合物，采用气相色谱-电子捕获检测器（ GC-ECD）检测具有较高的灵敏度，但由于拟除虫菊酯类农药分子量较大，其灵敏度显著低于有机氯，使得各类化合物进行分类检测的流程长、分析效率低。本文通过优选分析色谱柱和进样口温度等条件，利用气相色谱的色谱柱程序升压功能实现了多类别24种农药残留的快速、准确测定。实验中以正己烷为溶剂进行液液萃取，Florisil固相萃取柱净化，选择有机氯专用色谱柱（ RTX-CLPesticides 2）进行分析，GC-ECD仪器在0.5~6000 ng/mL浓度范围内呈线性，方法检出限为1.00~12.00 ng/L，低、中、高三个浓度水平的加标回收率分别为80.3%~116%、79.9%~117%、85.7%~102%，相应的精密度（RSD，n=7）为1.5%~6.8%、1.3%~7.6%、1.1%~6.8%。本方法选用的有机氯专用色谱柱（ RTX-CLPesticides 2）对多组分、多类别目标化合物有更好的分辨率，较通用型色谱柱（ DB-5 MS ）更具分析优势；采用的色谱柱程序升压技术解决了拟除虫菊酯类化合物在气相色谱柱中停留时间过长而导致的低灵敏度、峰拖尾等技术难题。此方法灵敏、经济，分析通量高，可有效地同时分析多种类农药残留物质。
擬除蟲菊酯類、有機氯、百菌清等農藥均屬于電負性彊化閤物，採用氣相色譜-電子捕穫檢測器（ GC-ECD）檢測具有較高的靈敏度，但由于擬除蟲菊酯類農藥分子量較大，其靈敏度顯著低于有機氯，使得各類化閤物進行分類檢測的流程長、分析效率低。本文通過優選分析色譜柱和進樣口溫度等條件，利用氣相色譜的色譜柱程序升壓功能實現瞭多類彆24種農藥殘留的快速、準確測定。實驗中以正己烷為溶劑進行液液萃取，Florisil固相萃取柱淨化，選擇有機氯專用色譜柱（ RTX-CLPesticides 2）進行分析，GC-ECD儀器在0.5~6000 ng/mL濃度範圍內呈線性，方法檢齣限為1.00~12.00 ng/L，低、中、高三箇濃度水平的加標迴收率分彆為80.3%~116%、79.9%~117%、85.7%~102%，相應的精密度（RSD，n=7）為1.5%~6.8%、1.3%~7.6%、1.1%~6.8%。本方法選用的有機氯專用色譜柱（ RTX-CLPesticides 2）對多組分、多類彆目標化閤物有更好的分辨率，較通用型色譜柱（ DB-5 MS ）更具分析優勢；採用的色譜柱程序升壓技術解決瞭擬除蟲菊酯類化閤物在氣相色譜柱中停留時間過長而導緻的低靈敏度、峰拖尾等技術難題。此方法靈敏、經濟，分析通量高，可有效地同時分析多種類農藥殘留物質。
의제충국지류、유궤록、백균청등농약균속우전부성강화합물，채용기상색보-전자포획검측기（ GC-ECD）검측구유교고적령민도，단유우의제충국지류농약분자량교대，기령민도현저저우유궤록，사득각류화합물진행분류검측적류정장、분석효솔저。본문통과우선분석색보주화진양구온도등조건，이용기상색보적색보주정서승압공능실현료다유별24충농약잔류적쾌속、준학측정。실험중이정기완위용제진행액액췌취，Florisil고상췌취주정화，선택유궤록전용색보주（ RTX-CLPesticides 2）진행분석，GC-ECD의기재0.5~6000 ng/mL농도범위내정선성，방법검출한위1.00~12.00 ng/L，저、중、고삼개농도수평적가표회수솔분별위80.3%~116%、79.9%~117%、85.7%~102%，상응적정밀도（RSD，n=7）위1.5%~6.8%、1.3%~7.6%、1.1%~6.8%。본방법선용적유궤록전용색보주（ RTX-CLPesticides 2）대다조분、다유별목표화합물유경호적분변솔，교통용형색보주（ DB-5 MS ）경구분석우세；채용적색보주정서승압기술해결료의제충국지류화합물재기상색보주중정류시간과장이도치적저령민도、봉타미등기술난제。차방법령민、경제，분석통량고，가유효지동시분석다충류농약잔류물질。
High sensitivity is required to determine pyrethroids,organochlorines,chlorothalonil and chlorpyrifos by using Gas Chromatography-Micro-Electron Capture Detector( GC-μECD)due to their high electro-negativity. The sensitivity of pyrethroids,which have higher molecular weights,is much lower than organochlorines. Moreover,the efficiency of determination is very low by different analyses patterns. This problem has been solved by using a column pressure program,and 24 compounds were determined efficiently at the same time by optimizing column conditions and inlet temperature. The underground water sample was treated by liquid-liquid extraction,Florisil SPE cleanup and analyzed by RTX-CL Pesticides 2 with GC-μECD. The calibration curves for 24 compounds were linear in the range of 0. 5-6000 ng/mL,and the method detection limits were in the range of 1. 00-12. 00 ng/L. The matrix spiked experiments were studied at three different concentration levels. The mean recoveries for low,middle and high concentration were in the range of 80. 3% -116%,79. 9% -117% and 85. 7% -102% with precisions of 1. 5% -6. 8%,1. 3% -7. 6% and 1. 1% -6. 8%,respectively. Compared to common chromatographic column(DB-5MS), the special chromatographic column( RTX-CLPesticides 2 ) is more efficient for analyzing multiple targets and category compounds. The low sensitivity and peak tailing problem of pyrethroids caused by long residence time in column was solved by using a column pressure program. The method is sensitive,accurate,and economical and maintains a high flux,which is easy to determine multiple pesticide residues simultaneously.
