推扫富集胶束电动毛细管色谱法和紫外分光光度法测定血液灌流前后血清中百草枯浓度的比较  

Comparison of Sweeping-MEKC and UV Determination of Trace Paraquat in Serum Before & After Hemoperfusion

作　　者：赵燕燕[1] 刘会芳[2] 王丽娟[3] 郝丽娜[3] 耿兆辉[1] 

机构地区：[1]河北大学医学实验中心,保定071000 [2]河北大学卫生职业技术学院,保定071000 [3]河北大学药学院,保定071000

出　　处：《应用化学》2008年第9期1069-1072,共4页Chinese Journal of Applied Chemistry

基　　金：河北省科技攻关项目(05276101D-88;42761220);河北省中医药管理局资助项目(05015);河北大学人才引进项目(y2004039);河北大学自然科学基金(2005Y08)资助项目

摘　　要：比较了推扫富集胶束电动毛细管色谱法和紫外分光光度法对血清中百草枯的快速检测。确定了胶束电动毛细管色谱法中,血清样品用体积分数为10%三氯乙酸进行去蛋白处理,采用未涂层的熔硅弹性石英毛细管(48.5 cm×50μm,有效柱长40 cm),以50 mmol/L磷酸盐-80 mmol/L十二烷基硫酸钠(SDS)(pH=2.50)为缓冲溶液,分离电压22 kV,进样压力5 kPa,在600 s内富集倍数达到650倍,检测波长260 nm。在紫外分光光度法中,血清样品经体积分数为20%三氯乙酸去蛋白处理,50μL微量比色池,紫外检测波长257 nm。胶束电动毛细管色谱法对百草枯的检测限为0.002 mg/L,相对标准偏差RSD为2.95%;紫外分光光度法对百草枯的检测限为0.01 mg/L,相对标准偏差RSD为2.50%。A micellar electrokinetic chromatography （MEKC） method based on on-line sweeping technique and ultraviolet spectrophotometry （UV） were compared for a fast determination of paraquat concentration in serum. For MEKC, the blood sample pretreatment required only the precipitation of protein contents by 10% trichloroacetic acid. In the running buffer of 50 mmoL/L phosphate and 80 mmoL/L sodium dodecyl sulfate （SDS） （pH = 2. 5 ） , the paraquat in the sample was successfully detected within 600 s, in a uncoated fusedsilica capillary column（48.5 cm × 50μm, effective length 40 cm） at a voltage of 22 kV, and a injection pressure of 5 kPa, with UV detection at 260 nm. For UV, the sample was deproteinizated by 20% trichloracetic acid, 50 μL microcell, the determination wavelength was 257 nm. Through the comparative analysis it shows that although ultraviolet spectrophotometry surpassed Sweeping-MEKC in the linear correlation coefficient and the reproduction of quantity, the limit of detection of UV was inferior to that of Sweeping-MEKC. The determitatiom limit of the former is lower, so it is applicable to the determination of the paraquat concentration in serum before and after hemoperfusion.

关 键 词：胶束电动毛细管色谱 在线推扫富集技术 紫外分光光度法 血液灌流 百草枯 血药浓度 

分 类 号：O655.9[理学—分析化学]