氯虫苯甲酰胺在菜薹中的残留及消解动态研究
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摘要
为确保氯虫苯甲酰胺的安全使用,制定在菜薹中的最大残留限量以及评价其在菜薹上的消解趋势、残留水平、对环境的污染情况,本文建立了氯虫苯甲酰胺在菜薹上残留的分散固相萃取-液相色谱串联质谱法,并用该方法研究5%氯虫苯甲酰胺悬浮剂在菜薹上的残留变化及消解动态,完成氯虫苯甲酰胺在菜薹中限量标准补点试验。样品经乙腈提取, PSA和GCB净化,质谱多反应监测扫描,基质匹配标准曲线外标法定量。在0.02～1 mg/L范围内具有良好的线性关系, r=0.997 4, 0.05～0.2 mg/kg添加水平下平均回收率为98.6%～103.8%,相对标准偏差(RSD)为2.3%～7.0%,最低检出浓度为0.05 mg/kg。在1年3地(北京、山东、浙江)的消解动态试验中,氯虫苯甲酰胺在菜薹上的消解半衰期t 1/2分别为3.55、 2.74和4.13 d,表明氯虫苯甲酰胺在菜薹上的消解速度较快;在1年6地(北京、山东、四川、广西、湖北、浙江)最终残留试验中,采用5%氯虫苯甲酰胺悬浮剂,分别按照推荐剂量(41.25 g a.i/hm~2)和推荐剂量的1.5倍(61.875 g a.i/hm~2)施药2～3次,施药间隔7 d,距末次施药5 d、 7 d、 10 d时,收获菜薹中的氯虫苯甲酰胺残留量(最大值1.130 mg/kg)低于我国规定其他芸薹类蔬菜的最大允许残留限量(MRL)值(2 mg/kg)。
引文
[1]吴玉娥,李静,郑坤明,等.UPLC-HRMS法探究氯虫苯甲酰胺在水稻植株中的内吸传导特性[J].农药,2017,56(3):176-179.
[2]LIU Y,ZHANG H,HE F,et al.Combined toxicity of chlorantraniliprole,lambda-cyhalothrin,and imidacloprid to the silkworm Bombyx mori(Lepidoptera:Bombycidae)[J].Environmental Science&Pollution Research,2018,25(23):22 598-22 605.
[3]VIJAYASREE V,BAI H,NASEEMA B S,et al.Persistence and effects of processing on reduction of chlorantraniliprole residues on cowpea fruits[J].Bulletin of Environmental Contamination&Toxicology,2013,90(4):494-498.
[4]刘刚.氯虫苯甲酰胺原药产品登记企业达到4家[J].农药市场信息,2018(13):28.
[5]KAR A,MANDAL K,SINGH B.Environmental fate of chlorantraniliprole residues on cauliflower using QuEChERS technique[J].Environmental Monitoring&Assessment,2013,185(2):1 255-1 263.
[6]LAI T,SU J.Effects of chlorantraniliprole on developmen and reproduction of beet armyworm,Spodoptera exigua(Hübner)[J].Journal of Pest Science,2011,84(3):381-386.
[7]国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[8]杨玉霞,莫仁甫,周其峰,等.氯虫苯甲酰胺在果蔗及其土壤中残留分析方法[J].西南农业学报,2016(11):2 643-2 647.
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[10]PAN X,DONG F,XU J,et al.Simultaneous determination of chlorantraniliprole and cyantraniliprole in fruits,vegetables and cereals using ultra-high-performance liquid chromatography-tandem mass spectrometry with the isotope-labelled internal standard method[J].Analytical&Bioanalytical Chemistry,2015,407(14):4 111-4 120.
[11]KILJANEK T,NIEWIADOWSKA A,SEMENIUK S,et al.Multi-residue method for the determination of pesticides and pesticide metabolites in honeybees by liquid and gas chromatography coupled with tandem mass spectrometry-Honeybee poisoning incidents[J].Journal of Chromatography A,2016,1 435(4):100-114.
[12]马婧玮,马欢,安莉,等.QuEChERS-高效液相色谱-串联质谱法测定主要谷物和油料作物中氯虫苯甲酰胺的残留[J].农药学学报,2018,20(1):129-134.
[13]李桂红,李二虎,张武,等.超高效液相色谱串联质谱测定果蔬中氯虫苯甲酰胺残留[J].世界农药,2018,40(3):58-61,64.
[14]XU P J,REN Y,ZHOU Z G,et al.Determination of chlorantraniliprole in vegetables,fruits and grains by SPE clean-up and LC-UV[J].Chromatographia,2010,72(7-8):763-766.
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[16]李红红,王彦辉,韦典,等.氯虫苯甲酰胺在甘蔗及土壤中的残留消解动态[J].农药学学报,2016,18(1):101-106.
[17]DONG F,XU J,LIU X,et al.Determination of Chlorantraniliprole Residues in Corn and Soil by UPLC-ESI-MS/MS and Its Application to a Pharmacokinetic Study[J].Chromatographia,2011,74(5-6):399-406.
[18]吴玉娥.氯虫苯甲酰胺在水稻上的残留分析和消解动态研究[D].贵阳:贵州大学,2017.
[19]陈国峰,刘峰,张晓波,等.氯虫苯甲酰胺在大豆和土壤中的残留及降解行为[J].农业环境科学学报,2016,35(5):894-900.
[20]李瑞娟,于建垒,宋国春,等.氯虫苯甲酰胺在甘蓝和土壤中的残留及消解动态[J].生态环境学报,2011,20(4):663-667.
[21]闫震,聂继云,徐国锋,等.超高效液相色谱-串联质谱法对比4种净化方式对不同色素含量基质中19种农药残留检测的影响[J].分析测试学报,2014,33(9):1 000-1 009.
[2]LIU Y,ZHANG H,HE F,et al.Combined toxicity of chlorantraniliprole,lambda-cyhalothrin,and imidacloprid to the silkworm Bombyx mori(Lepidoptera:Bombycidae)[J].Environmental Science&Pollution Research,2018,25(23):22 598-22 605.
[3]VIJAYASREE V,BAI H,NASEEMA B S,et al.Persistence and effects of processing on reduction of chlorantraniliprole residues on cowpea fruits[J].Bulletin of Environmental Contamination&Toxicology,2013,90(4):494-498.
[4]刘刚.氯虫苯甲酰胺原药产品登记企业达到4家[J].农药市场信息,2018(13):28.
[5]KAR A,MANDAL K,SINGH B.Environmental fate of chlorantraniliprole residues on cauliflower using QuEChERS technique[J].Environmental Monitoring&Assessment,2013,185(2):1 255-1 263.
[6]LAI T,SU J.Effects of chlorantraniliprole on developmen and reproduction of beet armyworm,Spodoptera exigua(Hübner)[J].Journal of Pest Science,2011,84(3):381-386.
[7]国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[8]杨玉霞,莫仁甫,周其峰,等.氯虫苯甲酰胺在果蔗及其土壤中残留分析方法[J].西南农业学报,2016(11):2 643-2 647.
[9]MALHAT F M.Determination of Chlorantraniliprole residues in grape by high-performance liquid chromatography[J].Food Analytical Methods,2012,5(6):1 492-1 496.
[10]PAN X,DONG F,XU J,et al.Simultaneous determination of chlorantraniliprole and cyantraniliprole in fruits,vegetables and cereals using ultra-high-performance liquid chromatography-tandem mass spectrometry with the isotope-labelled internal standard method[J].Analytical&Bioanalytical Chemistry,2015,407(14):4 111-4 120.
[11]KILJANEK T,NIEWIADOWSKA A,SEMENIUK S,et al.Multi-residue method for the determination of pesticides and pesticide metabolites in honeybees by liquid and gas chromatography coupled with tandem mass spectrometry-Honeybee poisoning incidents[J].Journal of Chromatography A,2016,1 435(4):100-114.
[12]马婧玮,马欢,安莉,等.QuEChERS-高效液相色谱-串联质谱法测定主要谷物和油料作物中氯虫苯甲酰胺的残留[J].农药学学报,2018,20(1):129-134.
[13]李桂红,李二虎,张武,等.超高效液相色谱串联质谱测定果蔬中氯虫苯甲酰胺残留[J].世界农药,2018,40(3):58-61,64.
[14]XU P J,REN Y,ZHOU Z G,et al.Determination of chlorantraniliprole in vegetables,fruits and grains by SPE clean-up and LC-UV[J].Chromatographia,2010,72(7-8):763-766.
[15]MALHAT F,ABDALLAH H,Hegazy I.Dissipation of Chlorantraniliprole in Tomato Fruits and Soil[J].Bulletin of Environmental Contamination&Toxicology,2012,88(3):349-351.
[16]李红红,王彦辉,韦典,等.氯虫苯甲酰胺在甘蔗及土壤中的残留消解动态[J].农药学学报,2016,18(1):101-106.
[17]DONG F,XU J,LIU X,et al.Determination of Chlorantraniliprole Residues in Corn and Soil by UPLC-ESI-MS/MS and Its Application to a Pharmacokinetic Study[J].Chromatographia,2011,74(5-6):399-406.
[18]吴玉娥.氯虫苯甲酰胺在水稻上的残留分析和消解动态研究[D].贵阳:贵州大学,2017.
[19]陈国峰,刘峰,张晓波,等.氯虫苯甲酰胺在大豆和土壤中的残留及降解行为[J].农业环境科学学报,2016,35(5):894-900.
[20]李瑞娟,于建垒,宋国春,等.氯虫苯甲酰胺在甘蓝和土壤中的残留及消解动态[J].生态环境学报,2011,20(4):663-667.
[21]闫震,聂继云,徐国锋,等.超高效液相色谱-串联质谱法对比4种净化方式对不同色素含量基质中19种农药残留检测的影响[J].分析测试学报,2014,33(9):1 000-1 009.