固相萃取-高效液相色谱法测定甘蔗和土壤中二甲四氯的残留量  被引量:9

Determination of MCPA residue in sugarcane and soil by solid-phase extraction and high-performance liquid chromatography

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作  者:傅强[1] 杨仁斌[1] 徐浩然[1] 廖海玉[1] 杨周宁[1] 

机构地区:[1]湖南农业大学资源环境学院,湖南长沙410128

出  处:《湖南农业大学学报(自然科学版)》2011年第5期554-557,共4页Journal of Hunan Agricultural University(Natural Sciences)

基  金:农业部农药检定所项目(NCR09091)

摘  要:建立了固相萃取-高效液相色潜法(SPE—HPLC)测定甘蔗和土壤中二甲四氯残留量。样品采用0.04mol/LNaOH提取,中性氧化铝固相萃取柱净化,HPLC—UV检测。二甲四氯在0.05-10mg/L线性关系良好(R2=0.9993);最低检出浓度为0.01mg/kg,添加水平为0.05、0.1、1.0mg/kg时,甘蔗和土壤中回收率为82.2%~89.1%,变异系数小于10%。在甘蔗植株中,二甲四氯的消解半衰期为1.78~2.69d;土壤样品中,二甲四氯的消解半衰期为2.40~3.64d。An analytical method was developed to extract and determine 2-methyl-4-chlorophenoxyacetic acid(MCPA) residue in sugarcane and soil using solid-phase extraction and high-performance liquid chromatography (SPE-HPLC). The MCPA residue in sugarcane and soil was dissolved in 0.04 mol/L sodium hydroxide aqueous solution, and purified through basic alumina-SPE column. Then the sample was detected by HPLC-UV. The method could be used to determine the MCPA residue in sugarcane and soil with fine linear relationship (R2=0.999 3) when the concentration range of MCPA was 0.05-10 mg/L and the limit of detection was 0.01 mg/kg. The recovery rates of MCPA from sugarcane and soil fortified with MCPA at 0.05,0.1,1.0 mg/kg were 82.2%-89.1% and 84.0%-85.7% respectively, with relative standard deviation 〈 10%. The results showed that the half-life of degradation for MCPA was 1.78-2.69 d in sugarcane, 2.40-3.64 d in soil.

关 键 词:二甲四氯 甘蔗 土壤 固相萃取 高效液相色谱 

分 类 号:S482.49[农业科学—农药学]

 

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