胶束电动毛细管色谱推扫富集测定蜂蜜中残留的杀虫脒和单甲脒  

Determination of chlordimeform and semiamitraz chloride in honey by micellar electrokinetic capillary chromatography with sweeping

作　　者：石杰[1] 陈冠华[1] 童明珠[1] 吴娴[1] 王坤[1] 

机构地区：[1]江苏大学食品与生物工程学院,江苏镇江212013

出　　处：《河北科技大学学报》2011年第5期421-425,445,共6页Journal of Hebei University of Science and Technology

基　　金：教育部高等学校博士学科点专项科研基金资助项目(20093227110010);江苏大学科研基金资助项目(08JDG001);江苏高校优势学科建设工程资助项目

摘　　要：建立了胶束电动毛细管色谱推扫富集测定蜂蜜中杀虫脒和单甲脒残留的分析新方法,对影响分离度和峰高的诸因素进行了选择。获得的最佳分离和富集条件如下:30mmol/L硼酸盐-20mmol/L十二烷基硫酸钠-20%(体积分数)甲醇运行缓冲溶液(pH值为9.67),进样量为10kV×90s,分离电压为20kV。在此优化条件下,杀虫脒和单甲脒的富集倍数分别为1 100和1 000倍,线性范围为0.03～0.25mg/L,检出限为0.88μg/kg和0.62μg/kg,加标回收率为91.8%～100.6%和90.5%～102.6%。该方法满足相关标准中的残留限量要求,可用于蜂蜜中杀虫脒和单甲脒农药残留的检测。A new assay of micellar electrokinetic capillary chromatography with sweeping was developed to determine chlordimeform and semiamitraz chloride in honey.The factors affecting resolution and peak height were studied.The optimum condition for separation and enrichment is determined as that the running buffer consists of 30 mmol/L borate,20 mmol/L sodium dodecyl sulfate and 20%（V/V） methanol whose pH is adjusted to 9.67.The sample is injected at 10 kV for 90 s,and the separation voltage is 20 kV.Under the optimum condition,the peak enrichment factors of chlordimeform and semiamitrazchloride are 1 100 and 1 000;the linear dynamic range is 0.03~0.25 mg/L;the detection limits and the average recoveries of spiked sample are 0.88 μg/kg and 91.8%~100.6% for chlordimeform,and 0.62 μg/kg and 90.5%~102.6% for semiamitraz chloride,respectively.The assay can meet the requirements of determination of maximum residue limits regulated by a number of countries and organizations,and can be applied to determine the residues in honey.

关 键 词：杀虫脒 单甲脒 胶束电动毛细管色谱 推扫 

分 类 号：O657.8[理学—分析化学]