露地和大棚条件下鱼藤酮和印楝素在黄瓜和土壤中的残留及消解动态
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摘要
拟建立一种高效液相色谱检测黄瓜和土壤中鱼藤酮和印楝素残留的方法,并比较分析鱼藤酮和印楝素在露地和大棚黄瓜和土壤中的残留及消解动态。按照农药登记残留田间试验施药标准操作规程,设计了2.5%鱼藤酮乳油84.375 g/hm~2(推荐高剂量的1.5倍)和0.3%印楝素乳油40.50 g/hm~2(推荐高剂量的10倍)在露地和大棚各施药1次,施药后1、6 h和1、2、3、5、7、10、14 d分别采样检测,再将二者按推荐剂量56.25、4.05 g/hm~2和1.5倍推荐剂量84.375、6.075 g/hm~2分别施药2、3次,施药间隔6 d,距离末次施药3、5、7 d采样测定。结果表明,鱼藤酮和印楝素的消解动态均符合一级动力学方程,鱼藤酮在黄瓜和土壤中的半衰期分别为1.45、2.36 d (露地)和1.74、2.62 d(大棚),印楝素在黄瓜和土壤中的半衰期分别为1.11、1.86 d(露地)和1.36、2.18 d(大棚);采收期距最后一次施药3～7 d时,露地和大棚采收的黄瓜样品中未检出印楝素,鱼藤酮的最高残留量分别为0.136 8、0.203 1 mg/kg,均低于我国规定的鱼藤酮在甘蓝中的最大残留限量(MRL)0.5 mg/kg,此时收获的黄瓜食用安全。鱼藤酮和印楝素于大棚条件下使用时在黄瓜和土壤中的原始沉积量均明显大于露地条件的相应值,与露地条件下相比更难降解,降解半衰期更长。
A method for detection of rotenone and azadirachtin residues in cucumber and soil by high performance liquid chromatography(HPLC) was established and applied in the analysis of cucumber and soil from open field and greenhouse.According to the standard operating procedures on pesticide registration residue field trials, rotenone and azadirachtin were sprayed for one time at the dosage of 84.375 g/ha(1.5 times of recommended dose) and 40.50 g/ha(10 times of recommended dose) in open field and greenhouse,respectively,and the cucumber and soil were sampled at 1,6 h and 1,2,3,5,7,10,14 d after application. In the other experiment, the cucumber and soil in open field and greenhouse were sampled at 3,5,7 d after the last application, which were sprayed for 2 or 3 times at an internal of 6 days at the recommended dosage(56.25 and 4.05 g/ha for rotenone and azadirachtin) and 1.5 times of the recommended dosage(84.375 and 6.075 g/ha for rotenone and azadirachtin).The results showed that the degradation dynamics of rotenone and azadirachtin in cucumber and soil all accorded with the first-order kinetics equation.The half-lives of rotenone were 1.45 d in cucumber and 2.36 d in soil in open field, and 1.74 d and 2.62 d in cucumber and soil in greenhouse condition,the half-lives of azadirachtin were 1.11 d in cucumber and 1.86 d in soil in open field,and 1.36 d and 2.18 d in cucumber and soil in greenhouse condition,respectively.The final residues of azadirachtin were not detected in the cucumber that was harvested at 3—7 d after the last application in open field and greenhouse,and the maximum residues of rotenone were 0.136 8、0.203 1 mg/kg in cucumber,which were all below the maximum residue limit(MRL) 0.5 mg/kg in cabbage set in China,and the cucumber harvested at this time was safe for human consumption.Contrasting the data,it could be concluded that the initial residue concentrations of rotenone and azadirachtin in cucumber and soil in greenhouse were always higher than those in open field,and their half-lives in greenhouse were longer than those in open field,which implied that rotenone and azadirachtin in greenhouse were more slow to be degraded than in open field.
A method for detection of rotenone and azadirachtin residues in cucumber and soil by high performance liquid chromatography(HPLC) was established and applied in the analysis of cucumber and soil from open field and greenhouse.According to the standard operating procedures on pesticide registration residue field trials, rotenone and azadirachtin were sprayed for one time at the dosage of 84.375 g/ha(1.5 times of recommended dose) and 40.50 g/ha(10 times of recommended dose) in open field and greenhouse,respectively,and the cucumber and soil were sampled at 1,6 h and 1,2,3,5,7,10,14 d after application. In the other experiment, the cucumber and soil in open field and greenhouse were sampled at 3,5,7 d after the last application, which were sprayed for 2 or 3 times at an internal of 6 days at the recommended dosage(56.25 and 4.05 g/ha for rotenone and azadirachtin) and 1.5 times of the recommended dosage(84.375 and 6.075 g/ha for rotenone and azadirachtin).The results showed that the degradation dynamics of rotenone and azadirachtin in cucumber and soil all accorded with the first-order kinetics equation.The half-lives of rotenone were 1.45 d in cucumber and 2.36 d in soil in open field, and 1.74 d and 2.62 d in cucumber and soil in greenhouse condition,the half-lives of azadirachtin were 1.11 d in cucumber and 1.86 d in soil in open field,and 1.36 d and 2.18 d in cucumber and soil in greenhouse condition,respectively.The final residues of azadirachtin were not detected in the cucumber that was harvested at 3—7 d after the last application in open field and greenhouse,and the maximum residues of rotenone were 0.136 8、0.203 1 mg/kg in cucumber,which were all below the maximum residue limit(MRL) 0.5 mg/kg in cabbage set in China,and the cucumber harvested at this time was safe for human consumption.Contrasting the data,it could be concluded that the initial residue concentrations of rotenone and azadirachtin in cucumber and soil in greenhouse were always higher than those in open field,and their half-lives in greenhouse were longer than those in open field,which implied that rotenone and azadirachtin in greenhouse were more slow to be degraded than in open field.
引文
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[12] 王世英.鱼藤酮和呋虫胺在多种蔬菜中的消解规律及影响因素研究[D].广州:华南农业大学,2016.
[13] 王苏宁,李冠华,李有志,等.固相萃取-高效液相色谱法检测上海青(Brassica chinensis L.)中鱼藤酮的残留动态[J].农药,2012,51(4):278-280.
[14] 杨晓云,黄其亮,江腾辉,等.印楝素在甘蓝及土壤中的消解动态[J].华南农业大学学报,2017,38(4):37-40.
[15] CABONI P,SARAIS G,ANGIONI A,et al.Fate of azadirachtin A and related azadirachtoids on tomatoes after greenhouse treatment[J].Journal of Environmental Science and Health(Part B),2009,44(6):598-605.
[16] SARAIS G,ANGIONI A,LAI F,et al.Persistence of two neem formulations on peach leaves and fruit:Effect of the distribution[J].Journal of Agricultural and Food Chemistry,2009,57(6):2457-2461.
[17] 周颖,安莹,燕传勇,等.超高效液相色谱-串联质谱法测定茶叶中印楝素A和B的残留量[J].理化检验(化学分册),2016,52(11):1292-1296.
[18] 唐艳梅,黎其万,刘宏程,等.固相萃取-高效液相色谱测定水果中印楝素残留量[J].农药,2011,50(1):53-54,60.
[19] 罗应兰,刘宏程.超声波固相萃取-高效液相色谱法同时测定茶叶中印楝素及类似物残留量[J].农药,2016,55(12):915-917.
[20] 中华人民共和国农业部.农药残留试验准则:NY/T 788—2004[S].北京:中国农业出版社,2004.
[21] 丁悦,孙星,汪佳蕾,等.露地和大棚条件下啶虫脒在黄瓜和土壤中的残留及消解动态[J].农药学学报,2014,16(1):110-114.
[22] 中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部.食品安全国家标准食品中农药最大残留限量:GB 2763—2016[S].北京:中国标准出版社,2016.
[2] 郑坤明,贾贵飞,龚谨,等.毒氟磷在大棚和露地西瓜和土壤中的残留消解动态[J].农药,2018,57(8):575-577,592.
[3] 黄兰淇,马琳,占绣萍,等.露地和大棚条件下噻虫嗪和啶虫脒在青菜中的残留及消解动态[J].农药,2018,57(1):42-45.
[4] 谢显传,张少华,王冬生,等.露地和大棚条件下阿维菌素在蔬菜作物上的残留消解动态比较[J].中国农业科学,2008,41(10):3399-3404.
[5] 任红,柯用春,许如意,等.大棚和露地条件下3种农药在冬种豇豆上的残留消解动态[J].南方农业学报,2012,43(11):1688-1691.
[6] 周游,张宁,黄其亮,等.鱼藤酮在甘蓝上的残留消解动态研究[J].西南农业学报,2013,26(2):587-590.
[7] CABONI P,SHERER T B,ZHANG N,et al.Rotenone,deguelin,their metabolites,and the rat model of parkinson’s disease[J].Chemical Research in Toxicology,2004,17(11):1540-1548.
[8] XUAN T D,EIJI T,HIROYUKI T,et al.Evaluation on phytotoxicity of neem (Azadirachta indica.A.Juss) to crops and weeds[J].Crop Protection,2004,23:335-345.
[9] ZHOU Y,ZHANG N,WANG K,et al.Dissipation and residue of rotenone in cabbage and soil under field conditions[J].Bulletin of Environmental Contamination and Toxicology,2013,91(2):251-255.
[10] CATTEAU L,LAUTIE E,KONE O,et al.Degradation of rotenone in yam bean seeds (Pachyrhizus sp.) through food processing[J].Journal of Agricultural and Food Chemistry,2013,61(46):11173-11179.
[11] 徐志英,任莉,陈小军,等.2.5%鱼藤酮微胶囊悬浮剂在普通白菜上的消解特性[J].中国蔬菜,2018(11):64-67.
[12] 王世英.鱼藤酮和呋虫胺在多种蔬菜中的消解规律及影响因素研究[D].广州:华南农业大学,2016.
[13] 王苏宁,李冠华,李有志,等.固相萃取-高效液相色谱法检测上海青(Brassica chinensis L.)中鱼藤酮的残留动态[J].农药,2012,51(4):278-280.
[14] 杨晓云,黄其亮,江腾辉,等.印楝素在甘蓝及土壤中的消解动态[J].华南农业大学学报,2017,38(4):37-40.
[15] CABONI P,SARAIS G,ANGIONI A,et al.Fate of azadirachtin A and related azadirachtoids on tomatoes after greenhouse treatment[J].Journal of Environmental Science and Health(Part B),2009,44(6):598-605.
[16] SARAIS G,ANGIONI A,LAI F,et al.Persistence of two neem formulations on peach leaves and fruit:Effect of the distribution[J].Journal of Agricultural and Food Chemistry,2009,57(6):2457-2461.
[17] 周颖,安莹,燕传勇,等.超高效液相色谱-串联质谱法测定茶叶中印楝素A和B的残留量[J].理化检验(化学分册),2016,52(11):1292-1296.
[18] 唐艳梅,黎其万,刘宏程,等.固相萃取-高效液相色谱测定水果中印楝素残留量[J].农药,2011,50(1):53-54,60.
[19] 罗应兰,刘宏程.超声波固相萃取-高效液相色谱法同时测定茶叶中印楝素及类似物残留量[J].农药,2016,55(12):915-917.
[20] 中华人民共和国农业部.农药残留试验准则:NY/T 788—2004[S].北京:中国农业出版社,2004.
[21] 丁悦,孙星,汪佳蕾,等.露地和大棚条件下啶虫脒在黄瓜和土壤中的残留及消解动态[J].农药学学报,2014,16(1):110-114.
[22] 中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部.食品安全国家标准食品中农药最大残留限量:GB 2763—2016[S].北京:中国标准出版社,2016.