分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
12期
1444-1447,1451
,共5页
毛细管电泳-电化学发光%钌联吡啶%百草枯%茶叶%离子对固相萃取
毛細管電泳-電化學髮光%釕聯吡啶%百草枯%茶葉%離子對固相萃取
모세관전영-전화학발광%조련필정%백초고%다협%리자대고상췌취
capillary electrophoresis-electrochemiluminescence%tris(2,2-bipyridyl)ruthenium(Ⅱ)%paraquat%tea%ion-pair solid-phase extraction
基于农药百草枯对钌联吡啶-三丙胺(TPA)体系的电化学发光具有显著的抑制作用,建立了毛细管电泳-间接电化学发光检测茶叶中残留农药百草枯的新方法.讨论了初始电位、钌联吡啶和TPA浓度、进样电压、进样时间、运行缓冲溶液的浓度与pH值等条件对百草枯检测灵敏度的影响.确定最佳实验条件为1.20 V初始电压、0.7 mmol/L钌联吡啶、0.6 mmol/L TPA、9 kV进样电压、9 s进样时间、35 mmol/L磷酸盐(pH 8.5)为运行缓冲溶液.在优化实验条件下,百草枯浓度在5×10~(-7) 5×10~(-5)mol/L范围内呈良好线性(相关系数为0.994 5),检出限为9.4×10~(-8) mol/L.对5×10~(-5) mol/L百草枯标准溶液连续测定5次,相对峰高与迁移时间的相对标准偏差分别为3.7%和2.1%.该方法对2.0×10~(-6)、1.0×10~(-5) mol/L百草枯标样的萃取回收率分别为74%和83%,相对标准偏差分别为15%、4.2%(n=5).
基于農藥百草枯對釕聯吡啶-三丙胺(TPA)體繫的電化學髮光具有顯著的抑製作用,建立瞭毛細管電泳-間接電化學髮光檢測茶葉中殘留農藥百草枯的新方法.討論瞭初始電位、釕聯吡啶和TPA濃度、進樣電壓、進樣時間、運行緩遲溶液的濃度與pH值等條件對百草枯檢測靈敏度的影響.確定最佳實驗條件為1.20 V初始電壓、0.7 mmol/L釕聯吡啶、0.6 mmol/L TPA、9 kV進樣電壓、9 s進樣時間、35 mmol/L燐痠鹽(pH 8.5)為運行緩遲溶液.在優化實驗條件下,百草枯濃度在5×10~(-7) 5×10~(-5)mol/L範圍內呈良好線性(相關繫數為0.994 5),檢齣限為9.4×10~(-8) mol/L.對5×10~(-5) mol/L百草枯標準溶液連續測定5次,相對峰高與遷移時間的相對標準偏差分彆為3.7%和2.1%.該方法對2.0×10~(-6)、1.0×10~(-5) mol/L百草枯標樣的萃取迴收率分彆為74%和83%,相對標準偏差分彆為15%、4.2%(n=5).
기우농약백초고대조련필정-삼병알(TPA)체계적전화학발광구유현저적억제작용,건립료모세관전영-간접전화학발광검측다협중잔류농약백초고적신방법.토론료초시전위、조련필정화TPA농도、진양전압、진양시간、운행완충용액적농도여pH치등조건대백초고검측령민도적영향.학정최가실험조건위1.20 V초시전압、0.7 mmol/L조련필정、0.6 mmol/L TPA、9 kV진양전압、9 s진양시간、35 mmol/L린산염(pH 8.5)위운행완충용액.재우화실험조건하,백초고농도재5×10~(-7) 5×10~(-5)mol/L범위내정량호선성(상관계수위0.994 5),검출한위9.4×10~(-8) mol/L.대5×10~(-5) mol/L백초고표준용액련속측정5차,상대봉고여천이시간적상대표준편차분별위3.7%화2.1%.해방법대2.0×10~(-6)、1.0×10~(-5) mol/L백초고표양적췌취회수솔분별위74%화83%,상대표준편차분별위15%、4.2%(n=5).
Based on a remarkable inhibited effect of paraquat on tris(2,2-bipyridyl)-ruthenium(Ⅱ)-tripropylamine(TPA) system,a new method for the determination of herbicide residue paraquat in tea was developed by capillary electrophoresis with indirect electrochemiluminescence detection.The tea samples was extracted by C18 ion-pair soild-phase extraction(SPE) column using acidic methanol as eluate.Influence of several factors such as initial potential,concentration of Ru(bpy)_3~(2+) and TPA,injection voltage and time,concentration and pH value of running buffer on detection sensitivity was investigated.The optimized conditions were as follows:initial potential:1.2 V,concentration of Ru(bpy)_3~(2+):0.7 mmol/L,concentration of TPA:0.6 mmol/L,injection voltage:9 kV,injection time:9 s,running buffer:35 mmol/L PBS buffer(pH 8.5).Under the optimized conditions,the calibration curve was linear in the range of 5×10~(-7)-5×10~(-5) mol/L for paraquat with a correlation coefficient of 0.994 5.The detection limit was 9.4×10~(-8) mol/L,and the relative standard deviations of ECL intensity and migration time for 5×10~(-5) mol/L paraquat(n=5) were 3.7% and 2.1%,respectively.The proposed method was applied to the determination of paraquat residue in tea.The extraction recoveries were 74% and 83% for paraquat of 2.0×10~(-6) and 1.0×10~(-5) mol/L,respectively,and the RSD values were 15% and 4.2%(n=5),respectively.
