多残留分析技术及其在PRAESS模型验证中的应用.docVIP

多残留分析技术及其在PRAESS模型验 证中的应用 孔祥吉张雪梅周军英韦笑王娜程燕单正军 环境保护部南京环境科学研究所国家环境保护农药环境评价与污染控制重点实验室江苏省计量科学研 环境保护部南京环境科学研究所 国家环境保护农药 环境评价与污染控制重点实验室 江苏省计量科学研 究院南京信息工程大学 摘要： ［目的］建立水环境中农药多残留的快速分析技术，为农药水生生态风险评价提 供技术支撑。［方法］采用固相萃取-气相色谱-质谱联用方法分析地表水屮10种 高风险稻田农药（毒死蝉、硫丹、灭多威、莠去津、烟喀磺隆、氟乐灵、百菌清、 苯醸甲环哇、二嗪磷、氯鼠菊酯等）的残留状况，对比固相萃取小柱、洗脱溶剂 等因素对回收效率的影响。［结果］釆用500 mg的HLB小柱、丙酮-乙酸乙酯-二 氯甲烷（体积比1 ： 1 ： 1）作为洗脫溶剂，GC/MS （SIM模式）测定地表水中10 种农药，最低检出限（L0D）在0. 005°. 1 u g/L,方法回收率在79%*16%o釆用该 方法验证PRAESS稻田-地表水模型及场景，测试质量浓度（l?83ug/L）与模型 预测质量浓度（2?32ug/L）有较高的拟合水平，后期测试质量浓度与模型估算 值有较大差异。［结论］多残留分析技术简便易行，PREASS模型仍有待于进一步 修正和完善。 关键词： I占I相萃取;气质联用;农药多残留分析;PREASS模型齡证; 作者简介：孔祥吉（1979—），男，博士，副研究员，主要研究方向为农用化学 品的测试技术与环境行为。E-ma订:kxj@nies. orgo 收稿日期：2017-06-12 Research on the Multi-residue Analysis Technique and Application in Validating of PRAESS KONG Xiang-ji ZHANCJCue-mei ZHOU Jun-ying WEI Xiao WANG Na CHENG Yan SHAN Zheng-jun Nanjing Institute of Environmental Sciences, MEP; Jiangsu Institute of Metrology; Nanjing University of Information science Technology; Abstract： [Aims] The aims were to establish the analysis techniques for pesticides multi-residues, and provide technical support for the ecological risk assessment on the pesticides. [Methods] The SPE_GC_MS technique was adopt in the analysis of 10 high risk pcsticidc residues in surface water, which was used in rice field, that were chlorpyrifos, endosulfan, methomyl, atrazine, nicosulfuron, trifluralin, chlorothalonil, difenoconazole, diazinon and cypermethrin. The effects of different type of SPE column and elution sol vents on recoveri es were discussed. [ResuIts] The operation con ditions were the IILB car tridge of 500 mg, and the mixed elution sol vent of acetone, ethyl acetate and dichloromethane （1 ： 1 ： 1, by vol） and SIM mode of GC-MS. The detec table residues level range for the 10 pesticides was between 0. 005 and 0. 1 u g/L, and recoveries were 79-116%. The analysis method was adopted in the validation of PRAESS mode in the rice_surface waiter model and scene. It was indica