摘要
利用超声萃取提取和组合填料层析柱净化样品,建立了黄瓜百菌清和毒死蜱含量的气相色谱（GC）检测方法.市售黄瓜经研磨后,称取10 g,加入50 mL V（正己烷）∶V（丙酮）=60∶40溶液,超声波提取30 min,再经直径为1 cm的层析柱（自下而上为无水硫酸钠＋5 cm硅胶＋1 cm氧化铝）分离,用25 mL V（正己烷）∶V（丙酮）=90∶10混合淋洗液洗脱,收集淋洗液,定容至25 mlL后测定.百菌清乖毒死蜱标准溶液的气相色谱分析出峰时间分别为出9.438和10.597,黄瓜样品中两种农药出峰时间分别为9.452和10.611.百菌清和毒死蜱在黄瓜样品中回收率在92.5％～104％之间;在质量浓度范围80～400 μg/L内线性关系良好,线性回归系数分别为0.999和0.998;最低检测限分别为28 μg/L和33 μg/L,能满足农药残留分析的要求.
A gas chromatography （GC） determination of chlorothalonil （CHT） and chlopyrifos （CHP） in cucumber has been established,combined with ultrasonic extraction and alumina and silica gel chromatographic column purification.After cucumbers bought from market were cleaned and grinded,about 10 g mashed cucumber were mixed with 50 mL mixture solution of V （n-hexane） and V （acetone） =60 ∶ 40,and extracted with ultrasonic wave for 30 min.After that,purification was conducted by a 1-cm-diameter chromatographic column filled with some anhydrous sodium sulfate,5 cm silica gel,and 1cm aluminium oxide from bottom to top.At last,the analytes were eluviated by 25 mL mixture solution of V （n-hexane） and V （acetone） =90 ∶10.The effluent was collected and set the volume to 25 mL,then determined by GC.The peak time of CHT and CHP in standard solutions appeared at 9.438 and 10.597,while in the cucumber sample,the peak time of the two pesticides was 9.452 and 10.611,respectively.The average recoveries of CHT aud CHP in samples were in range of 92.5％ -104 ％.Good linear relationships existed iu the concentration range of 80 - 400 μg/L,with linear regression coefficients of 0.999 and 0.998 for CHT and CHP,and the limits of detection were 28μg/L and 33 μg/L,respectively.The method met the analytical requirements of the pesticide residue.
出处
《浙江工业大学学报》
CAS
2014年第3期330-333,共4页
Journal of Zhejiang University of Technology
基金
国家973重点基础研究发展规划基金资助项目(2009CB119006)
关键词
分析方法
黄瓜
百菌清
毒死蜱
analytical method
cucumber
chlorolthalonil
chlorpyrifos
