多残留分析技术及其在PRAESS模型验证中的应用  

Research on the Multi-residue Analysis Technique and Application in Validating of PRAESS

作　　者：孔祥吉[1,2] 张雪梅 周军英[1,2] 韦笑[4] 王娜 程燕[1,2] 单正军[1,2] 

机构地区：[1]环境保护部南京环境科学研究所,南京210042 [2]国家环境保护农药环境评价与污染控制重点实验室,南京210042 [3]江苏省计量科学研究院,南京210023 [4]南京信息工程大学,南京210042

出　　处：《农药》2017年第12期912-915,925,共5页Agrochemicals

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中10种高风险稻田农药(毒死蜱、硫丹、灭多威、莠去津、烟嘧磺隆、氟乐灵、百菌清、苯醚甲环唑、二嗪磷、氯氰菊酯等)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]采用500 mg的HLB小柱、丙酮-乙酸乙酯-二氯甲烷(体积比1∶1∶1)作为洗脱溶剂,GC/MS(SIM模式)测定地表水中10种农药,最低检出限(LOD)在0.005~0.1μg/L,方法回收率在79%~116%。采用该方法验证PRAESS稻田-地表水模型及场景,测试质量浓度(1.83μg/L)与模型预测质量浓度(2.32μg/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。[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 pesticide 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 solvents on recoveries were discussed. [Results] The operation conditions were the HLB cartridge of 500 mg, and the mixed elution solvent of acetone, ethyl acetate and dichloromethane（1∶1∶1, by vol） and SIM mode of GC-MS. The detectable residues level range for the 10 pesticides was between 0.005 and 0.1 μg/L, and recoveries were 79-116%. The analysis method was adopted in the validation of PRAESS mode in the rice-surface water model and scene. It was indicated that the highest concentration of chlorpyrifos was 1.83 μg/L tested in the field, which fit well with the peak value of 2.32 μg/L predicted by the PRAESS Risk Prediction Model, however, it has great difference between the detection values and estimates from follow-up samples.[Conclusions] The pesticide multi-residue analysis techniques were simple and convenient, and PREASS model need more verification and improvement.

关 键 词：固相萃取 气质联用 农药多残留分析 PREASS模型验证 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]