乙氧呋草黄和苯嗪草酮在甜菜中的残留和降解
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摘要
[目的]建立了甜菜、植株及土壤中乙氧呋草黄和苯嗪草酮的残留分析方法,并采用田间试验方法研究了乙氧呋草黄和苯嗪草酮在甜菜植株和土壤中的消解动态及其在甜菜、甜菜植株和土壤中的残留规律。[方法]样品用乙腈-水溶液振荡提取,经分散固相萃取净化,超高效液相色谱-串联质谱测定。[结果]乙氧呋草黄在甜菜、甜菜植株和土壤中的平均回收率为81.5%～99.1%,变异系数在4.8%～14.0%之间,最低检测质量分数为0.02 mg/kg;苯嗪草酮在甜菜、甜菜植株和土壤中的平均回收率为93.8%～104.9%,变异系数在1.1%～5.7%之间,最低检测质量分数为0.02 mg/kg。[结论]2016—2017年在黑龙江省田间残留试验表明:按照一级动力学反应模型拟合,乙氧呋草黄和苯嗪草酮在土壤中的半衰期分别为1.4～5.0、3.5～5.5 d,乙氧呋草黄和苯嗪草酮在植株中未拟合出半衰期;甜菜最终样品中乙氧呋草黄的残留量均<0.02 mg/kg,苯嗪草酮的残留量均<0.02 mg/kg。
[Aims] A method for determination of ethofumesate and metamitron in sugarbeet, plant and soil was developed. Meanwhile, the dissipation and residue characteristics of ethofumesate and metamitron were investigated by field experiments. [Methods] The samples were extracted with acetonitrile and water, cleaned up by dispersive solid phase extraction, determined by UPLC-MS/MS, and quantified by the external standard method. [Results] The minimum detectable concentrations of ethofumesate and metamitron in sugarbeet were 0.02 mg/kg. The recoveries of ethofumesate in sugarbeet, plant and soil were 81.5-99.1 % with the relative standard deviations of 4.8-14.0%. The recoveries of metamitron in sugarbeet, plant and soil were 93.8-104.9 % with the relative standard deviations of1.1-5.7%. [Conclusions] The field experiments revealed that the residue dissipation dynamics of ethofumesate and metamitron in soil conformed to the first order kinetics reaction model. The half-lives of ethofumesate and metamitron in soil were 1.4-5.0 and 3.5-5.5 d, respectively. The half-lives in sugarbeet plant were not calculated. The final residues of ethofumesate and metamitron were <0.02 mg/kg both in sugarbeet and soil.
[Aims] A method for determination of ethofumesate and metamitron in sugarbeet, plant and soil was developed. Meanwhile, the dissipation and residue characteristics of ethofumesate and metamitron were investigated by field experiments. [Methods] The samples were extracted with acetonitrile and water, cleaned up by dispersive solid phase extraction, determined by UPLC-MS/MS, and quantified by the external standard method. [Results] The minimum detectable concentrations of ethofumesate and metamitron in sugarbeet were 0.02 mg/kg. The recoveries of ethofumesate in sugarbeet, plant and soil were 81.5-99.1 % with the relative standard deviations of 4.8-14.0%. The recoveries of metamitron in sugarbeet, plant and soil were 93.8-104.9 % with the relative standard deviations of1.1-5.7%. [Conclusions] The field experiments revealed that the residue dissipation dynamics of ethofumesate and metamitron in soil conformed to the first order kinetics reaction model. The half-lives of ethofumesate and metamitron in soil were 1.4-5.0 and 3.5-5.5 d, respectively. The half-lives in sugarbeet plant were not calculated. The final residues of ethofumesate and metamitron were <0.02 mg/kg both in sugarbeet and soil.
引文
[1]陈国建.黑龙江省甜菜化学除草方法浅析[J].农业与技术,2017,37(8):9.
[2]顾林玲.三嗪酮类除草剂——苯嗪草酮[J].现代农药,2016,15(4):51-54.
[3]李小敏,蒋爱琴,徐方豪,等.除草剂乙氧呋草黄的合成[J].精细石油化工,2001(1):57-60.
[4]李小敏,华万森,陆路德.除草剂乙氧呋草黄的合成与表征[J].南京理工大学学报,2000,24(3):215-218.
[5]王萍.手性农药乙氧呋草黄对映体在生物体和环境中的活性及立体选择性行为的研究(博士论文)[D].北京:中国农业大学,2005.
[6]徐欣媛.两种手性除草剂在动物体内的选择性行为研究(博士论文)[D].北京:中国农业大学,2014.
[7]陆阳,陶京朝,周志莲.苯嗪草酮的合成新工艺[J].化工中间体,2010(6):49-54.
[8]蒋晓帆,赵昊昱.苯嗪草酮的合成[J].化学世界,2015(10):626-629.
[9]刘兵,陈其平.苯嗪草酮700 g/L水悬浮剂的配方研究[J].农药科学与管理,2012,33(7):16-20.
[10]潘洪吉,张群峰,李常平.苯嗪草酮原药的液相色谱分析方法[J].农药科学与管理,2000,21(2):4-24.
[11]WALORCZYK S,DROZ觶DZ觶Y SKI D,KIERZEK R.Determination of Pesticide Residues in Samples of Green Minor Crops by Gas Chromatography and Ultra Performance Liquid Chromatography Coupled to Tandem Quadrupole Mass Spectrometry[J].Talanta,2015,132:197-204.
[12]REJCZAK T,TUZIMSKI T.Qu ECh ERS-based Extraction with Dispersive Solid Phase Extraction Clean-up Using PSA and Zr O2-Based Sorbents for Determination of Pesticides in Bovine Milk Samples by HPLC-DAD[J].Food Chemistry,2017,217:225-233.
[2]顾林玲.三嗪酮类除草剂——苯嗪草酮[J].现代农药,2016,15(4):51-54.
[3]李小敏,蒋爱琴,徐方豪,等.除草剂乙氧呋草黄的合成[J].精细石油化工,2001(1):57-60.
[4]李小敏,华万森,陆路德.除草剂乙氧呋草黄的合成与表征[J].南京理工大学学报,2000,24(3):215-218.
[5]王萍.手性农药乙氧呋草黄对映体在生物体和环境中的活性及立体选择性行为的研究(博士论文)[D].北京:中国农业大学,2005.
[6]徐欣媛.两种手性除草剂在动物体内的选择性行为研究(博士论文)[D].北京:中国农业大学,2014.
[7]陆阳,陶京朝,周志莲.苯嗪草酮的合成新工艺[J].化工中间体,2010(6):49-54.
[8]蒋晓帆,赵昊昱.苯嗪草酮的合成[J].化学世界,2015(10):626-629.
[9]刘兵,陈其平.苯嗪草酮700 g/L水悬浮剂的配方研究[J].农药科学与管理,2012,33(7):16-20.
[10]潘洪吉,张群峰,李常平.苯嗪草酮原药的液相色谱分析方法[J].农药科学与管理,2000,21(2):4-24.
[11]WALORCZYK S,DROZ觶DZ觶Y SKI D,KIERZEK R.Determination of Pesticide Residues in Samples of Green Minor Crops by Gas Chromatography and Ultra Performance Liquid Chromatography Coupled to Tandem Quadrupole Mass Spectrometry[J].Talanta,2015,132:197-204.
[12]REJCZAK T,TUZIMSKI T.Qu ECh ERS-based Extraction with Dispersive Solid Phase Extraction Clean-up Using PSA and Zr O2-Based Sorbents for Determination of Pesticides in Bovine Milk Samples by HPLC-DAD[J].Food Chemistry,2017,217:225-233.