固液萃取-高效液相色谱-串联质谱法同时测定土壤中阿特拉津及其降解产物

建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时检测土壤中阿特拉津及其降解产物残留的分析方法。样品以甲醇-水(4∶1,V/V)作为提取溶剂,使用涡旋振荡提取,采用HPLC-MS/MS法进行测定,外标法定量。在0.01、0.2和5.0mg/kg三个添加浓度水平下,阿特拉津及其降解产物的平均回收率在73.7%~104.7%之间,相对标准偏差为0.4%~5.1%;阿特拉津,羟基阿特拉津在土壤样品中的方法检出限均0.045μg/kg,而脱乙基阿特拉津、脱乙基脱异丙基阿特拉津及脱异丙基阿特拉津在土壤样品中的方法检出限则分别为0.090、0.45和0.90μg/kg。本方法的灵敏度较高,且简便、快速,能较好的解决目标物极性差别大及样品基质对检测结果的干扰等问题,可以满足土壤中阿特拉津及其降解产物残留检测的需要。

Simultaneous Determination of Atrazine and Its Degradation Products in Soil Using Vortex Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

A sensitive method was developed to simultaneously determine atrazine(ATZ) and its major degradation products including hydroxyatrazine (HA),desethylatrazine (DEA),desisopropylatrazine (DIA) and desethyl-desisopropylatrazine(DAA) in soil.The compounds were extracted by vortexing soil samples with a methanol and water(4∶1,V/V) solution and measured using high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS).At three spiked levels(0.01,0.2,5.0 mg/kg),the average recoveries of the analytes from soil samples ranged from 73.7％ to 104.7％ with relative standard deviations from 0.4％ to 5.1％.The limits of detection in soil were ＜0.045 μg/kg for ATZ and HA,0.090 μg/kg for DEA,0.45 μg/kg for DAA and 0.90 μg/kg for DIA.The method is rapid,cost-effective and can be applied to assess contamination of soils with atrazine and its degradation products.