气相色谱-三重四级杆串联质谱法测定土壤中氟啶虫酰胺、氟吡菌酰胺、唑虫酰胺、杀虫脲和氟虫脲  

Determination of flutamide,flupirimide,azolomide,chlorfenuron and flufenuron in soil by gas chromatography tandem mass spectrometry

作　　者：李珊 孙志洪 郭伟伟 路瑞娟 LI Shan;SUN Zhihong;GUO Weiwei;LU Ruijuan(Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China;Cangzhou Ecological Environment Monitoring Center,Cangzhou 061000,China;Cangzhou Academy of Ecological Environment Protection,Cangzhou 061000,China)

机构地区：[1]河北省沧州生态环境监测中心,河北沧州061000 [2]沧州市生态环境监控中心,河北沧州061000 [3]沧州市生态环境保护科学研究院,河北沧州061000

出　　处：《中国测试》2022年第6期64-68,共5页China Measurement & Test

摘　　要：建立一种加速溶剂萃取(ASE)结合气相色谱-三重四级杆串联质谱(GC-MS/MS)检测土壤中农药残留的分析方法。土壤样品粉碎过筛,与适量的硅藻土混合均匀放入萃取池中,以丙酮∶乙酸乙酯(体积比:1∶1)混合溶剂进行萃取。萃取液经氨基固相萃取柱净化后,在HP-5ms(30 m×0.25 mm,0.25μm)毛细管柱进行分离,气相色谱质谱中以多反应监测模式扫描测试,外标法定量分析。结果表明5种农药残留在0.02~2.0μg/mL范围内线性关系良好,相关系数均大于0.99;检出限均在0.006~0.012 mg/kg之间,在三个浓度的添加水平下,平均加标回收率均在87.8%~106.4%之间,精密度RSD在1.86%~3.82%(n=6)。该方法提取效率高,定性定量结果准确,可用于土壤中农药残留的监测。An effective method was developed to determine pesticides residues in soil by accelerated solvent extractioncoupled with gas chromatography-tandem mass spectrometry(ASE-GC-MS/MS).Soil sample was crushed and screened,mixed with appropriate amount of diatomite and put into the extraction tank.,acetone:ethyl acetate(V:V,1:1)solution was selected as the extraction solvent.Afterpurified onCarb/NH;solid phase extraction(SPE)column,The residues were separated on the HP-5MS(30 m×0.25 mm,0.25μm)capillary column,analyzed by GC-MS/MS with multiple reactionmonitoring mode,and quantified by external standard method.5 pesticidesshowed good linear relationships in the concentration range 0.02-4.0μg/mL,with correlation coefficients all above 0.99.The detection limits were in the rangge 0.006-0.012 mg/kg.Average recoveries were ranged from 87.8%to 106.4%.Relative standard deviation(RSD)was 1.86%-3.82%(n=6).This method has high extraction efficiency,accurate qualitative and quantitative results,and can be used for monitoring pesticide residues in soil.

关 键 词：加速溶剂萃取 气相色谱-三重四级杆串联质谱 土壤 氟啶虫酰胺 残留 

分 类 号：TB9[一般工业技术—计量学]