基质分散萃取-高效液相色谱法对菠菜中噻虫胺残留的检测  

Determination of Clothianidin Residue in Spinach by QuEChERS-HPLC

作　　者：李广领[1] 谷珊山[1] 刘博[1] 陈锡岭[1] 

机构地区：[1]河南科技学院资源与环境学院,河南新乡453003

出　　处：《湖北农业科学》2016年第2期465-468,共4页Hubei Agricultural Sciences

基　　金：河南省教育厅科学技术研究重点项目(13B210003);河南省高等学校重点科研项目(15A210024);河南科技学院研究生创新基金项目(2014CX057)

摘　　要：研究确立了乙腈为分散萃取溶剂,以羧基化双壁碳纳米管(DWCNTs-COOH)和石墨化碳黑(GCB)为基质分散材料的菠菜(Spinacia oleracea L.)样品中噻虫胺残留基质分散萃取前处理方法,建立并优化了乙腈等度洗脱的HPLC残留样品外标定量方法。结果表明,优化色谱条件下,噻虫胺标准样品的色谱保留时间为6.258 min,在0.05~100 mg/L范围内与对应色谱峰积分面积线性响应良好,回归方程为y=4.948 2x-1.316 9(R^2=0.999 7),噻虫胺在菠菜样品中0.1、0.5和5.0 mg/kg 3个水平的添加回收率均在85%以上,各添加水平的相对标准偏差均小于7%,该色谱条件下仪器检出限为0.052 7μg/L,方法的最低检测量为0.015 mg/kg。表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足噻虫胺在菠菜中的残留定量检测要求。A liquid chromatography-ultraviolet detector（HPLC-UVD） method was established for clothianidin residue in spinach by dispersive solid phase extraction using acetonitrile as extraction solvent, double carbon nano tubes（DWCNT＇s） and graphitized carbon（GCB） as sorbent. The results showed that under the optimal conditions, the retention time of clothianidin was 6.25 minute,the calibration curves showed good linearity（y =4.948 2x-1.316 9,R2=0.999 7） from 0.005 -100 mg / L mass concentration of clothianidin.The recovery rates were determined in spinach blank spiked at 0.1,0.5 and 5.0 mg / kg and the overall recovery rates were over 85%,with a relative standard deviation（RSD） less than 7%.The detection limit of clothianidin was 0.052 7 μg and the limit of quantification was 0.015 mg / kg in spinach. So the obtained sample pretreatment method and the residue sample detection method was simple process, good treatment effect, low operation cost,and stable reliability,and it＇s suitable for the determination of clothianidin residues in spinach.

关 键 词：基质分散萃取 碳纳米管 菠菜(Spinacia OLERACEA L.) 噻虫胺 高效液相色谱法 

分 类 号：O657.7[理学—分析化学] S636.1[理学—化学]