气相色谱-串联质谱法同时测定食用菌种植土壤中5种常用三氮苯类除草剂的含量  

Simultaneous Determination of Five Common Triazene Herbicides in Edible Fungus Planting Soil by Gas Chromatography Tandem Mass Spectrometry

作　　者：范睿 孙志洪 路瑞娟 郭伟伟 倪洁 FAN Rui;SUN Zhihong;LU Ruijuan;GUO Weiwei;NI Jie(Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061001,China;Cangzhou Academy of Ecological and Environmental Protection,Cangzhou 061001,China;Cangzhou Ecological and Environmental Monitoring Centre,Cangzhou 061001,China;Hengshui Ecological Environment Monitoring Center of Hebei Province,Hengshui 053000,China)

机构地区：[1]河北省沧州生态环境监测中心,沧州061001 [2]沧州市生态环境保护科学研究院,沧州061001 [3]沧州市生态环境监控中心,沧州061001 [4]河北省衡水生态环境监测中心,衡水053000

出　　处：《理化检验（化学分册）》2023年第9期1032-1036,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：目前关于除草剂残留量测定的研究涉及的三氮苯类除草剂种类单一,不能全面考察土壤中三氮苯类除草剂微量残留的水平,基于此进行了题示研究。取10.0g预处理后的样品,加入约12g硅藻土混匀后,按设定的加速溶剂萃取程序于80℃萃取10min。萃取液经凝胶渗透色谱净化,洗脱液于50℃氮吹至近干,残渣用1mL体积比1∶2的丙酮-乙醇混合液涡旋溶解,采用气相色谱-串联质谱法(GC-MS/MS)同时测定滤液中西玛津、氰草津、莠去津、扑灭津和草达津等5种除草剂的含量。结果表明,5种除草剂的质量浓度在0.01~5.0mg·L^(-1)内与对应的峰面积呈线性关系,检出限(3S/N)为0.010~0.014 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为84.6%~103%。对0.1mg·L^(-1)空白土壤加标样品平行测定6次,测定值的相对标准偏差均小于3.0%。方法用于实际食用菌种植土壤样品的分析,其中莠去津的检出量分别为0.015,0.011mg·kg^(-1),扑灭津的检出量为0.020mg·kg^(-1)。The research on the determination of triazene herbicide residues involves a single type of herbicide at present,which could not comprehensively examine the level of trace triazene herbicide residues in soil.Therefore,the study mentioned by title was done.The pre-treated sample(10.0g)was taken,and about 12g of diatomite was added.After mixing well,the mixture was extracted at 80℃for 10 min according to the set accelerated solvent extraction procedure.The extraction solution was purified by gel permeation chromatography,and the eluent was blown to near dryness at 50℃by nitrogen.The residue was dissolved by 1mL of a mixture of acetone and ethanol at a volume ratio of 1∶2.Five herbicides in the filtrate,including simazine,cyanazine,atrazine,ipramazine,and oxalazine,were simultaneously determined by gas chromatography tandem mass spectrometry(GC-MS/MS).As shown by the results,linear relationships between values of peak area and mass concentration of five herbicides were found in the range of 0.01-5.0mg·L^(-1).with detection limits(3S/N)ranged from 0.010to 0.014mg·kg^(-1).Test for recovery was made by standard addition method,giving results in the range of 84.6%-103%.The 0.1mg·L^(-1) blank soil sample was parallel determined 6times,with RSDs of the determined values less than 3.0%.The method was applied to the analysis of soil samples from actual edible fungus planting soil samples,with detection amounts of 0.015,0.011mg·kg^(-1) for atrazine and 0.020mg·kg^(-1) for chlorpyrifos,respectively.

关 键 词：气相色谱-串联质谱法(GC-MS/MS) 土壤 除草剂 

分 类 号：O657.63[理学—分析化学]