HPLC Determination of Residual Carbamate Pesticides in Fruits and Vegetables with On-line Post-column Derivatization and Fluorescence Detection
摘 要
提出了具有在线柱后衍生流路及荧光检测器的高效液相色谱法测定了果蔬中6种氨基甲酸酯类农药.果蔬样品经匀浆后用乙腈萃取,经固相萃取柱纯化.用甲醇及二氯甲烷(1+99)混合溶剂作淋洗剂,淋出液经氮吹蒸干后用甲醇溶解,所得溶液供高效液相色谱分析.采用Carbamate Analysis柱(3.9 mm×150 mm,5 μm)作为固定相,并用不同比例配制的甲醇和水的溶液作为流动相进行梯度淋洗.在线柱后衍生化系在一反应器中进行,0.05 mol·L-1氢氧化钠溶液及衍生化试剂邻苯二甲醛溶液均以0.5 mL·min-1速率引入于反应器中.采用339 nm及445 nm分别作为荧光检测的激发波长和发射波长,测得6种农药的线性范围均在0.01~2.5 mg·L-1之间,其检出限(3S/N)在0.5~3.0 μg·kg-1之间.用标准加入法测得方法的回收率在86.4%~103.0%之间.
Abstract
Six residual carbamate pesticides in fruits and vegetables were determined by HPLC with on-line post-column derivatization and fluorescence detection.The sample was pounded,homogenized and extracted with acetonitrile,and purified by SPE column.The mixed solvent of methanol and dichloromethane(1+99) was used as eluant,and the eluates were collected and evaporated to dryness by N2-blowing.The residue was taken up with methanol and used for HPLC analysis.The Carbamate Analysis column (3.9 mm×150 mm,5 μm) was used as stationary phase and mixtures of methanol and H2O with various ratios were used as mobile phase in gradient elution.On-line post-column derivatization was carried out in the reactor into which 0.05 mol·L-1 NaOH solution and derivatizing agent,OPA solution were introduced at a flow-rate of 0.5 mL·min-1.Fluorescence detection was made at wavelengths of 339 nm (λex) and 445 nm (λem).Ranges of linearity for the 6 pesticides were found between 0.01-2.5 mg·L-1,with detection limits (3S/N) in the range of 0.5-3.0 μg·kg-1.Results of recovery test obtained were in the range of 86.4%-103.0%.
中图分类号 O652.63
所属栏目 工作简报
基金项目
收稿日期 2009/4/29
修改稿日期
网络出版日期
作者单位点击查看
备注程盛华(1980-),男,江西九江人,工程师,研究方向为食品中农药、兽药残留的检测分析.
引用该论文: CHENG Sheng-hua,TANG Bin,ZHENG Long,DING Li. HPLC Determination of Residual Carbamate Pesticides in Fruits and Vegetables with On-line Post-column Derivatization and Fluorescence Detection[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(7): 816~819
程盛华,唐斌,郑龙,丁丽. 在线柱后衍生-荧光检测-高效液相色谱法测定果蔬中残留氨基甲酸酯农药[J]. 理化检验-化学分册, 2010, 46(7): 816~819
被引情况:
【1】马睿,刘春玲, "顺序注射荧光光谱法测定环境水中痕量西维因",理化检验-化学分册 50, 421-424(2014)
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】宋学省.高效液相色谱法测定蔬菜中的氨基甲酸酯[J].吉林蔬菜,2005,3:50-52.
【2】刘敏,端裕树,宋苑苑,等.分散固相萃取-液相色谱-质谱检测蔬菜水果中氨基甲酸酯和有机磷农药[J].分析化学,2006,7(7):941-942.
【2】刘敏,端裕树,宋苑苑,等.分散固相萃取-液相色谱-质谱检测蔬菜水果中氨基甲酸酯和有机磷农药[J].分析化学,2006,7(7):941-942.
相关信息