30%病氰硝可湿性粉剂在烟草及土壤上的残留分析
摘要
病氰硝是贵州省精细化工试验研究中心研制的一种新型抗烟草花叶病毒的绿色新农药,具有高效、广谱、低毒等特点。本实验以病氰硝为研究对象进行了两年两地的残留分析实验。以超声波辅助丙酮/水混合溶剂超声提取、液—液萃取及柱层析净化,高效液相色谱仪测定烟草及土壤中病氰硝的残留量。方法的最小检出量为1.3 ng,病氰硝在烟草及土壤中的最低检测浓度均为0.08 mg/kg。土壤在0.08、0.80、4.00 mg/kg三个添加水平上,平均回收率为87.58%～105.96%,相对标准偏差2.1%～8.7%;烟叶在0.08、0.80、2.40 mg/kg三个添加水平上,平均回收率为92.61%～108.14%,相对标准偏差1.6%～5.4%。以上数据表明方法的准确度、精密度和灵敏度均达到农药残留检测的要求。
试验结果表明,病氰硝在土壤上半衰期为8.1～12.4 d;在烟草中半衰期为5.9～6.5 d。在500 g.a.i/ha、1000 g.a.i/ha的施药水平下,施药2或3次,每次间隔7d,结果表明:距最后一次施药21 d病氰硝在两年两地土壤中最终残留量均小于0.15 mg/kg,在烟草中最终残留量均小于0.80 mg/kg。该试验条件下,病氰硝的最终残留量与施药浓度、施药次数呈正相关,与采收间隔期呈负相关。
Bingqingxiao that has its characters of high effectiveness, low toxicity and broad spectrum is a new pesticide of resisting tobacco mosaic virus. In the paper two-year-residue-assignment of bingqingxiao was carried out in different place. The analytical method was developed for detecting bingqingxiao residues in tobacco. Residues were extracted with mixture solvents of acetone and water, cleaned by liquid-liquid extraction and Florisil column, then detected by HPLC. The minimum amount of detection was 1.3 ng. The detectable limit of concentration was 0.08mg/kg in tobacco and soil. The average recoveries at levels of 0.08 to 4.00 mg/kg were found to be in the range 87.58% to 105.96% With the RSD (relative standard deviations) of variations from 2.1% to 8.7% in soil. In tobacco, the average recoveries at levels of 0.08 to 2.40 mg/kg were found to be in the range 92.61% to 108.14% with the RSD of variations from 1.6% to 5.4%. The result showed that the accuracy and sensitivity of method meet the requirements of pesticide residue analysis.
The conclusion showed that the half-life of Bingqingxiao were 8.1～12.4 days in soil and 5.9～6.5 days in tobacco. Bingqingxiao were treated two and three and interval of 7 days with the dosages of 500g.a.i/ha and 1000g.a.i/haduing the growing season of tobacco .The terminal residues levels of Bingqingxioa in soil and tobacco were respectively less than 0.15mg/kg and 0.80mg/kg after Bingqingxiao being applicated for 21 days .There were positive relationship between residues and amount as well as times, and negative relationship between residues and the days from last application.
试验结果表明,病氰硝在土壤上半衰期为8.1～12.4 d;在烟草中半衰期为5.9～6.5 d。在500 g.a.i/ha、1000 g.a.i/ha的施药水平下,施药2或3次,每次间隔7d,结果表明:距最后一次施药21 d病氰硝在两年两地土壤中最终残留量均小于0.15 mg/kg,在烟草中最终残留量均小于0.80 mg/kg。该试验条件下,病氰硝的最终残留量与施药浓度、施药次数呈正相关,与采收间隔期呈负相关。
Bingqingxiao that has its characters of high effectiveness, low toxicity and broad spectrum is a new pesticide of resisting tobacco mosaic virus. In the paper two-year-residue-assignment of bingqingxiao was carried out in different place. The analytical method was developed for detecting bingqingxiao residues in tobacco. Residues were extracted with mixture solvents of acetone and water, cleaned by liquid-liquid extraction and Florisil column, then detected by HPLC. The minimum amount of detection was 1.3 ng. The detectable limit of concentration was 0.08mg/kg in tobacco and soil. The average recoveries at levels of 0.08 to 4.00 mg/kg were found to be in the range 87.58% to 105.96% With the RSD (relative standard deviations) of variations from 2.1% to 8.7% in soil. In tobacco, the average recoveries at levels of 0.08 to 2.40 mg/kg were found to be in the range 92.61% to 108.14% with the RSD of variations from 1.6% to 5.4%. The result showed that the accuracy and sensitivity of method meet the requirements of pesticide residue analysis.
The conclusion showed that the half-life of Bingqingxiao were 8.1～12.4 days in soil and 5.9～6.5 days in tobacco. Bingqingxiao were treated two and three and interval of 7 days with the dosages of 500g.a.i/ha and 1000g.a.i/haduing the growing season of tobacco .The terminal residues levels of Bingqingxioa in soil and tobacco were respectively less than 0.15mg/kg and 0.80mg/kg after Bingqingxiao being applicated for 21 days .There were positive relationship between residues and amount as well as times, and negative relationship between residues and the days from last application.
引文
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2.于康平,李泽方,徐韶康等.嘧菌酯的高效液相色谱分析[J].农药,2008,47(4):275-276
3.王丽颖,张国生.20%烯肟菌胺·戊唑醇悬浮剂高效液相色谱分析[J].农药,2004,43(9):417-418
4.申中兰,蔡继宝,高芸等.基质固相分散—加速溶剂萃取—气相色谱法检测土壤中有机氯农药残留[J].分析化学,2005,33(9):1318-1320
5.尹丰平,卢植新,林明珍等.气相色谱法测定嘧菌酯在黄瓜和土壤中的残留方法研究[J].农药科学与管理,2005,26(2):17-20
6.冯秀琼,汤庆勇.中草药种14种有机磷农药残留量同时测定-微波辅助提取法[J].农药学学报,2001,1(3):45-52
7.李久团主编.最新农药使用与残留检测标准实施手册[M].北京伯通电子出版社,北京,2002
8.朱莉萍,朱涛,潘玉香等.气相色谱法同时测定蔬菜及水果中多种农药残留量[J].分析化学研究报告,2008,36(7):999-1003
9.农业部农药检定所.农药残留量实用检测方法手册(第一卷)[M].中国农业科技出版社
10.孙洁,薄海波,韩舜愈.果蔬中嘧菌酯残留量的气相色谱分析研究[J].甘肃农业大学学报,2007,2(4)112-115
11.孙宝华,刘英闲,王培德.苯氧菌酯的高效液相色谱法测定[J].农药,2003,42(6):22-23
12.孙静.固相萃取法图区净化生物学建材中三类农药的实验研究[J].环境科学,1995,14(3):221-225
13.杜小刚,扬扬,金凤鸣等.超超声波萃取法测定茶叶中有机磷农药残留方法[J].江苏工业学院学报,2005,17(2):20-22
14.吴宪,李建中,胡继业等.GC法检测醚菌酯在黄瓜中的残留[J].环境化学,2005,24(4):24
15.赵利剑,杨亚玲,夏静.固相萃取技术的研究[J].四川化工 2005,3:21-25
16.张海霞,朱彭龄.固相萃取[J].分析化学,2000,28(9):172-118
17.张慧苹,宋宝安,王献友等.2-氰基丙烯酸酯类化合物的合成与抗病毒活性研究[J].中国化工学会农药专业委员会第十二届年会会议论文(西安).2005,95-98
18.张玉婷,郭永泽,邵辉等.50%醚菌酯水分散粒剂在苹果及土壤种的残留动态[J].农药,2008,47(9):668-669
19.范金志,张海科,马琳等.新杀菌剂唑菌酯原药的HPLC分析[J].四川师范大学学报,2008,31(3):348-340
20.杨曼君.农药残留的免疫方法[J].农药科学与管理,1996,60(4):20-22
21.杨依军,王勇,杨秀荣等.免疫分析技术在农药残留分析技术中的应用[J].华北农学报,2001,16(4):119-124
22.秦曙,乔雄梧,王霞等.应用GC—MS测定葡萄中的五种农药残留[J].分析测试学报,2004,9(23)增刊:242-244
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