氟吡菌胺和吡唑醚菌酯在葡萄和土壤中的残留分析  

Residual Analysis of Fluopicolide and Pyraclostrobin in Grape and Soil

作　　者：陈恒辉 龚道新[1,2] 王寒[1,2] 杨丽华[1,2] 熊胜 徐钰哲 CHEN Heng-hui;GONG Dao--xin;WANG Han;YANG Li-hua;XIONG Sheng;XU Yu-zhe(Hunan Agricultural University College of Resource and Environment,Changsha,410128,China;Hunan Agricultural University Instiute of Agricultural Environmental Protection,Changsha,410128,China)

机构地区：[1]湖南农业大学资源环境学院,长沙410128 [2]湖南农业大学农业环境保护研究所,长沙410128

出　　处：《农药》2019年第2期112-114,124,共4页Agrochemicals

摘　　要：[目的]建立高效液相色谱法同时检测葡萄、土壤中氟吡菌胺和吡唑醚菌酯残留的方法。[方法]葡萄和土壤样品均用乙腈提取,提取液用PSA及C18吸附剂分散固相萃取净化,高效液相色谱检测,外标法定量。[结果]方法的线性范围为0.05～5.00 mg/L,氟吡菌胺相关系数为1.0000,吡唑醚菌酯相关系数为0.9999;在0.05、0.50、2.00 mg/kg 3个添加水平下,葡萄中氟吡菌胺和吡唑醚菌酯的平均回收率分别为86.7%～97.8%和90.6%～95.6%,相对标准偏差分别为2.55%～8.49%和2.14%～7.80%,土壤中氟吡菌胺和吡唑醚菌酯的平均回收率分别为79.1%～93.6%和83.4%～98.9%,相对标准偏差分别为5.29%～6.78%、1.69%～7.34%;在上述检测条件下,氟吡菌胺的最小检出量(LOD)为0.1 ng,在葡萄和土壤中的最低检测浓度(LOQ)均为0.05 mg/kg;吡唑醚菌酯的最小检出量(LOD)为0.1 ng,在葡萄和土壤中的最低检测浓度(LOQ)均为0.05 mg/kg。[结论]该方法具有简单可靠,分析样品时间短,准确度、精密度和灵敏度符合农药残留分析要求等特点,可以用于同时检测葡萄、土壤上氟吡菌胺和吡唑醚菌酯的残留量。[Aims] A high performance liquid chromatography(HPLC) method for the simultaneous determination of fluopicolide and pyraclostrobin residues in grapes and soil was established. [Methods] Grape and soil samples were extracted with acetonitrile, and the extracts were purified by solid phase extraction with PSA and C18 adsorbents,detectedbyHPLCandquantified byexternalstandard method. [Results]The linearrange ofthe method was0.05-5.00 mg/L,the correlation coefficient of fluopicolide was 1.0000, the correlation coefficient of pyraclostrobin was 0.9999, and the average recoveries of fluopicolide and pyraclostrobin in grape ranged from 86.7 to 97.8% and 90.6 to 95.6% at the levels of 0.05, 0.50 and 2.00 mg/kg, respectively. The average recoveries of flupiramide and pyraclostrobin in soil ranged from 79.1 to 93.6% and 83.4 to 98.9% respectively with relative standard deviation(RSD) of 1.69-7.34%. The limit of detection(LOD) of fluopicolide was 0.1 ng, and the limit of quantitation(LOQ) in grape and soil was both 0.05 mg/kg.The limit of detection(LOD) of pyraclostrobin was 0.1 ng, and the limit of quantitation(LOQ) of pyraclostrobin in grape and soil was 0.05 mg/kg. [Conclusions] The method is simple, reliable and rapidly. The accuracy, precision and sensitivity meet the requirements of pesticide residue analysis. It can be used for the simultaneous determination of fluopicolide and pyraclostrobin residues in grape and soil.

关 键 词：氟吡菌胺 吡唑醚菌酯 葡萄 土壤 高效液相色谱 

分 类 号：TQ450.7[化学工程—农药化工]