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高效液相色谱-柱后衍生法测定东盟水果中氨基甲酸酯类农药残留 被引量:14

High-performance Liquid Chromatographic Method with Post-column Derivatization for the Determination of Carbamate Residues in ASEND Fruits
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摘要 建立了高效液相色谱-柱后衍生法测定东盟水果中氨基甲酸酯类农药残留。样品用乙腈提取,提取液经浓缩、氨基固相萃取小柱净化,甲醇-二氯甲烷(5∶95,V/V)洗脱。采用Agilent Eclipse XDB-C8柱(250×4.6mm,5μm),流动相为甲醇-水,梯度洗脱,流速1.0mL/min,柱温35.0℃。用荧光检测器对涕灭威亚砜、涕灭威砜、灭多威、三羟基克百威、涕灭威、克百威和甲萘威进行测定,外标法定量。结果表明,氨基甲酸酯类农药在0.05-5.00mg/L质量浓度范围内线性良好,相关系数在0.9991-0.9994之间,回收率为80.6%-107.7%,变异系数在0.5%-8.8%之间,方法的检出限为0.001-0.003mg/kg。 A high performance liquid chromatographic(HPLC)method with post-column derivatization for determining carbamate residues in ASEND fruits was established.The sample was extracted with acetonitrile,cleaned up by an aminopropy Bond Elut(NH2)SPE column,and eluted by methanol and dichloromethane(5∶95,V/V).The aldicarb sulfoxide,aldicarb sulfone,methomyl,3-hydroxycarbofuran,aldicarb,carbofuran and carbaryl were separated on an Agilent Eclipse XDB C8column(250×4.6mm,5μm)at35.0℃ by using agradient methyl alcohol-water system as mobile phase at a rate of 1.0mL/min.The detection wavelength was set atλex=330nm andλem =465nm,and the external standard method was used for quantitative analysis.The results showed that the linear ranges for 7carbamates were 0.01-5.00mg/L with correlation coefficients from 0.9991 to 0.9994.The average recoveries of carbamates were between 80.6%and 107.7%,with variation coefficients ranging from 0.5%to 8.8%.The limits of detection of this method were between 0.001mg/kg and 0.003mg/kg.
出处 《分析科学学报》 CAS CSCD 北大核心 2015年第4期589-592,共4页 Journal of Analytical Science
基金 农业部农垦局农产品质量追溯系统建设项目(No.(2011)C0107) 广西壮族自治区直属公益性科研院所基本科研项目(桂热研No.200904)
关键词 氨基甲酸酯类农药 高效液相色谱 水果 农药残留 荧光检测 Carbamates High liquid chromatography Fruits Residues Fluorescence detection
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