气质法测定大棚土壤中的9种有机磷农药  

GC/MS Method for Determination of 9 Organ Phosphorus Pesticide Residues in Soil of Greenhouse

作　　者：杨敬坡[1,2] 霍永伟 王文军[4] 陈晓轩 罗建美[5] 吴黎军 YANG Jingpo;HUO Yongwei;WANG Wenjun;CHEN Xiaoxuan;LUO Jianmei;WU Lijun(School of Environmental Science&Engineering,Hebei University of Science and Technology,Shijiazhuang 050018;Pollution Prevention Biotechnology Laboratory of Hebei Province,Shijiazhuang 050018;Hebei Utilization and Planning Istitute of land Resources,Shijiazhuang 050051;College of Automobile and Electronic Engineering,Baoding College,Baoding 071051;College of Land Resources and Rural-Urban Planning,Hebei GEO University,Shijiazhuang 050031;Department of Student Affairs,Handan University,Handan 056005)

机构地区：[1]河北科技大学环境科学与工程学院,石家庄050018 [2]河北省污染防治生物技术实验室,石家庄050018 [3]河北省国土资源利用规划院,石家庄050051 [4]保定学院汽车与电子工程学院,保定071051 [5]河北地质大学土地资源与城乡规划学院,石家庄050031 [6]邯郸学院学工部,邯郸056005

出　　处：《食品工业》2019年第9期242-245,共4页The Food Industry

基　　金：国家自然科学基金(41807157);河北省科技支撑计划项目(15273610D);河北科技大学16PT基金(2016PT43);河北省社会科学发展研究课题民生调研专项(201701410);河北省海洋局项目(HYJJDC201606)

摘　　要：建立气相色谱质谱法检测大棚蔬菜种植土壤中的9种有机磷类(毒死蜱、氧乐果、乙酰甲胺磷、马拉硫磷、乐果、甲基对硫磷、二嗪磷、三唑磷、治螟磷)农药的检测方法。样品经冰乙酸-乙腈溶液匀浆提取后,提取液经N-丙基乙二胺(PSA)、无水硫酸镁和C18进行分散萃取净化,浓缩后用丙酮定容至1 mL。经气相色谱-质谱仪定性定量检测,基质标准定量。结果表明, 9种有机磷类农药在0.05~5μg/m L范围内线性关系良好, R2均小于0.995;当加标浓度为0.5, 1.0和3.0 mg/kg时,得到的回收率范围为83.2%~98.2%;检出限为0.006~0.020 mg/kg;精密度RSD(n=6)为1.54%~4.23%。A GC/MS method for determining 9 organophosphorus pesticide residues(chlorpyrifos, omethoate, acephate, malathion, dimethoate, parathion-methyl, diazinon, triazophos, and sulfotep) in soil of greenhouse was established. Samples were homogenized and extracted by acetonitrile-glacial acetic acid, the extracted solution then purified by PSA, anhydrous magnesium and C18. Purified solution was diluted with acetone to 1 mL, then was filtered and detected qualitatively and quantitatively by GC/MS, and quantified by matrix-match standard solution. The result showed that concentration of 9 organophosphorus pesticide residues showed good linear relationships in the range of 0.05-5 μg/mL, and the correlation coefficients were all above 0.995. The detection limits of 9 organ phosphorus pesticides were 0.006-0.020 mg/kg and the average recoveries at 3 spiked level of 0.5, 1.0 and 3.0 μg/mL varied from 83.2% to 98.2%. The RSD of precision was 1.54%-4.23%(n=6), and the relative standard deviation(RSD) of repeatability of 9 pesticide residues was 1.04%-3.36%(n=6).

关 键 词：QUECHERS 气相色谱-质谱 大棚 土壤 有机磷农药 

分 类 号：R28[医药卫生—中药学]