马铃薯及土壤中霜脲氰残留量的高效液相色谱快速分析方法
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摘要
[目的]建立高效液相色谱方法快速测定马铃薯茎叶、块茎及其土壤中霜脲氰残留量的方法。[方法]样品经乙腈提取,NH2固相萃取小柱净化后,以乙腈-水为流动相,使用C18色谱柱,通过Waters 2695高效液相色谱-紫外检测器,在254 nm检测波长下对霜脲氰进行分析检测,面积外标法定量。[结果]在0.1、0.5、2.0 mg/kg 3个不同添加浓度水平下,马铃薯茎叶中平均回收率为78.0%~104.4%,相对标准偏差为2.7%~3.4%;马铃薯块茎中平均回收率为82.9%~94.7%,相对标准偏差为1.1%~2.3%;土壤中平均回收率为81.6%~91.8%,相对标准偏差为3.3%~5.4%。霜脲氰在浓度为0.05~2.00 mg/L时线性关系良好(r=0.999 8),最小检出量为0.06 ng,在马铃薯茎叶、块茎和土壤中的最低检测浓度均为10μg/kg。[结论]该方法简便、快捷、成本低、精密度好、准确率高,适用于马铃薯及其土壤中霜脲氰的大批量分析检测,是一种较为实用的检测方法。
[Objective] A rapid determination method was established for the residue of cymoxanil in potato stem leaf,tuber and soil by HPLC. [Method]The samples were extracted with acetonitrile and purified by NH2 solid-phase extraction column. Analysis and determination were conducted by Waters 2695 HPLC with C18 column and UV detector at 254 nm,and CH3 CN-H2 O was utilized as the mobile phase. The residues were quantified by area of external standard method. [Result] When the concentration levels were added at different levels of 0. 1,0. 5 and 2. 0 mg/kg,the average recoveries of residues were 78. 0%-104. 4% with RSD of 2. 7%-3. 4% in potato stem leaves,and82. 9%-94. 7% with RSD of 1. 1%-2. 3% in potato tubers,and 81. 6%-91. 8% with RSD of 3. 3%-5. 4% in soil. The linear relationship was obtained in the concentration that range from 0. 05 to 2. 00 mg/L for cymoxanil( r = 0. 999 8). The minimum detectable amount of cymoxanil was 0. 06 ng. The minimum detectable concentrations of cymoxanil was 10 μg/kg in potato stem leaf,tuber and soil. [Conclusion]This method has advantages of simple,rapid,low cost,good precision and high accuracy,which is a practical detection method for the large batch analysis of cymoxanil in potato and soil.
[Objective] A rapid determination method was established for the residue of cymoxanil in potato stem leaf,tuber and soil by HPLC. [Method]The samples were extracted with acetonitrile and purified by NH2 solid-phase extraction column. Analysis and determination were conducted by Waters 2695 HPLC with C18 column and UV detector at 254 nm,and CH3 CN-H2 O was utilized as the mobile phase. The residues were quantified by area of external standard method. [Result] When the concentration levels were added at different levels of 0. 1,0. 5 and 2. 0 mg/kg,the average recoveries of residues were 78. 0%-104. 4% with RSD of 2. 7%-3. 4% in potato stem leaves,and82. 9%-94. 7% with RSD of 1. 1%-2. 3% in potato tubers,and 81. 6%-91. 8% with RSD of 3. 3%-5. 4% in soil. The linear relationship was obtained in the concentration that range from 0. 05 to 2. 00 mg/L for cymoxanil( r = 0. 999 8). The minimum detectable amount of cymoxanil was 0. 06 ng. The minimum detectable concentrations of cymoxanil was 10 μg/kg in potato stem leaf,tuber and soil. [Conclusion]This method has advantages of simple,rapid,low cost,good precision and high accuracy,which is a practical detection method for the large batch analysis of cymoxanil in potato and soil.
引文
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[10]中华人民共和国农业部农药检定所,山西省农药重点实验室.农药残留试验准则:NY/T 788—2004[S].北京:中国农业出版社,2004:2-5.
[2]张娇艳,李东,刘文静,等.几种杀菌剂对黄瓜霜霉病的防效研究[J].世界农药,2015,37(1):45-47.
[3]李艳琼.5种杀菌剂对葡萄霜霉病的控制效果[J].甘肃农业大学学报,2011,46(6):62-65.
[4]吴承金,李大春,颜学明,等.五种药剂对马铃薯晚疫病的防治效果[J].湖北农业科学,2014,53(22):5419-5422.
[5]刘明洋,龚道新,任竞,等.葡萄和土壤中霜脲氰的残留分析方法[J].湖南农业大学学报(自然科学版),2009,35(2):195-199.
[6]王亚慧,侯志广,密东林,等.高效液相色谱法同时测定马铃薯及其土壤中的霜脲氰和嘧菌酯[J].农药,2014,53(11):815-817.
[7]何丽丽,徐应明,孙有光,等.复配剂中霜脲氰在马铃薯和土壤中残留动态研究[J].农业环境科学学报,2007,26(1):322-325.
[8]TELLIER F,FRITZ R,LEROUX P,et al.Metabolism of cymoxanil and analogs in strains of the fungus Botrytis cinerea using high-performance liquid chromatography and ion-pair high-performance thin-layer chromatography[J].Journal of chromatography B,2002,769(1):35-46.
[9]刘祥云,崔滢,杨艳.影响霜脲氰在土壤中降解的因素研究[J].广州化工,2014,42(8):101-103,120.
[10]中华人民共和国农业部农药检定所,山西省农药重点实验室.农药残留试验准则:NY/T 788—2004[S].北京:中国农业出版社,2004:2-5.