三氟苯嘧啶在水稻、土壤和田水中的残留分析方法
|
摘要
[目的]建立高效液相色谱法检测水稻(糙米、谷壳和植株)、土壤和田水中三氟苯嘧啶残留的方法。[方法]待测样品中的三氟苯嘧啶用乙腈提取,糙米、植株和谷壳用PSA及Carbon-GCB吸附剂分散固相萃取净化,高效液相色谱检测,外标法定量。[结果]方法的线性范围为0.1~20 mg/L,相关系数为0.9999;在0.05、0.2、1 mg/kg 3个添加水平下,糙米和土壤中的平均回收率分别为84.3%~98.4%和80.1%~96.2%,相对标准偏差分别为2.52%~8.9%和3.33%~7.41%。在0.1、1、5 mg/kg 3个添加水平下,植株和稻壳的平均回收率分别为90.1%~99.8%和93.5%~96.1%,相对标准偏差分别为1.56%~8.31%和4.29%~6.77%。在0.02、0.2、1 mg/kg 3个添加水平下,田水的平均回收率为81.5%~95.2%,相对标准偏差为3.39%~7.78%。在上述检测条件下,三氟苯嘧啶的最小检出量为2 ng。[结论]该方法简单可靠,灵敏度、准确度、精密度符合农药残留分析要求,可用于水稻、土壤和田水中三氟苯嘧啶的残留检测。
[Aims] A new method for analysis of triflumezopyrim residues in rice(rough rice, plant and hull), soil and field water by high performance liquid chromatograph was developed. [Methods] The samples were extracted with dichloromethane. The triflumezopyrim residues in rough rice, plant and hull were purified by PSA and Carbon-GCB,then separated with SHIMADZU LC-20 AT. Finally, the samples were detected by photodiode array detector of HPLC.[Results] The linear range of calibration curves was 0.1-20 mg/L and linear correlation coefficient was 0.9999. When the spiked levels were 0.05, 0.2 and 1.0 mg/L, the average recoveries of triflumezopyrimin in rough rice were 84.3-98.4%with relative standard deviations of 2.52-8.9%, the average recoveries of triflumezopyrim in soil were 80.1-96.2% with relative standard deviations of 3.33-7.41%. When the spiked levels were 0.1, 1.0 and 5.0 mg/kg, the average recoveries of triflumezopyrim in rice plant were 90.1-99.8% with relative standard deviations of 1.56-8.31%. The average recoveries of triflumezopyrim in rice hull were 93.5-96.1% with relative standard deviations of 4.29-6.77%. When the spiked levels were 0.02, 0.2 and 1.0 mg/kg, the average recoveries of triflumezopyrim in field water were 81.5-95.2%with relative standard deviations of 3.39-7.78%. Under these conditions, the limits of detection for triflumezopyrim were2.0 ng. [Conclusions] The method is simple and reliable, the sensitivity and precision meet with the requirement for pesticide residue analysis, which can be applied for analysis of triflumezopyrim residues in rice, soil and field water.
[Aims] A new method for analysis of triflumezopyrim residues in rice(rough rice, plant and hull), soil and field water by high performance liquid chromatograph was developed. [Methods] The samples were extracted with dichloromethane. The triflumezopyrim residues in rough rice, plant and hull were purified by PSA and Carbon-GCB,then separated with SHIMADZU LC-20 AT. Finally, the samples were detected by photodiode array detector of HPLC.[Results] The linear range of calibration curves was 0.1-20 mg/L and linear correlation coefficient was 0.9999. When the spiked levels were 0.05, 0.2 and 1.0 mg/L, the average recoveries of triflumezopyrimin in rough rice were 84.3-98.4%with relative standard deviations of 2.52-8.9%, the average recoveries of triflumezopyrim in soil were 80.1-96.2% with relative standard deviations of 3.33-7.41%. When the spiked levels were 0.1, 1.0 and 5.0 mg/kg, the average recoveries of triflumezopyrim in rice plant were 90.1-99.8% with relative standard deviations of 1.56-8.31%. The average recoveries of triflumezopyrim in rice hull were 93.5-96.1% with relative standard deviations of 4.29-6.77%. When the spiked levels were 0.02, 0.2 and 1.0 mg/kg, the average recoveries of triflumezopyrim in field water were 81.5-95.2%with relative standard deviations of 3.39-7.78%. Under these conditions, the limits of detection for triflumezopyrim were2.0 ng. [Conclusions] The method is simple and reliable, the sensitivity and precision meet with the requirement for pesticide residue analysis, which can be applied for analysis of triflumezopyrim residues in rice, soil and field water.
引文
[1]英君伍,雷光月,宋玉泉,等.三氟苯嘧啶的合成与杀虫活性研究[J].现代农药,2017,16(2):14-16.
[2]杨吉春,王秀丽,杨帆.2013年公开的新农药品种[J].农药,2014,53(2):123-125.
[3]RATTAN R S,SINGH V,PAN Y F,et al.Du PontTM PyraxaltTM(DPX-RAB55;Triflumezopyrim):Low Sensitivity to Natural Enemies of Rice Ecosystem[C]//International Iupac Conference on“Agrochemicals Protecting Crop,Health and Natural Environment New Chemistries for Phytomedicines and Crop Protection Chemicals.2016:61.
[4]杨光.杜邦三氟苯嘧啶将获我国首登[J].农药市场信息,2016(8):606.
[5]JR H C,CORDOVA D,ZHANG Wen-ming,et al.Mesoionic Insecticides:A Novel Class of Insecticides that Modulate Nicotinic Acetylcholine Receptors[J].Pest Management Science,2017,73(4):796-806.
[6]CORDOVA D,BENNER E A,SCHROEDER M E,et al.Mode of Action of Triflumezopyrim:A Novel Mesoionic Insecticide Which Inhibits the Nicotinic Acetylcholine Receptor[J].Insect Biochemistry&Molecular Biology,2016(74):32.
[7]ZHANG Wen-ming,JR C W H,PAHUTSKI T F,et al.Mesoionic Pyrido[1,2-a]Pyrimidinones:Discovery of Triflumezopyrim as a Potent Hopper Insecticide 1[J].Bioorganic&Medicinal Chemistry Letters,2017,27(1):16-20.
[8]SINGH V,TEIXEIRA L,VINCENT D,et al.Triflumezopyrim(Pyraxalt TM)-A New Approach to Rice Plant Hopper Management in Asia Pacific[C]//Xxv International Congress of Entomology.2016.
[9]唐涛,叶波,刘雪源,等.多靶标杀虫剂—三氟苯嘧啶混配剂对水稻害虫的田间防治效果[J].植物保护,2016,42(6):202-207.
[10]SINGH V,TEIXEIRA L,LEIGHTY R M,et al.Du PontTM PyraxaltTM(DPX-RAB55;Triflumezopyrim):A novel chemistry for Rice Planthopper Management in Asia Pacific[C]//International Iupac Conference on“Agrochemicals Protecting Crop,Health and Natural Environment New Chemistries for Phytomedicines and Crop Protection Chemicals.2016.
[11]俞建忠,谢昀,姜宜飞,等.Triflumezopyrim 10%悬浮剂高效液相色谱分析方法研究[J].农药科学与管理,2015,36(3):49-51.
[12]中华人民共和国农业部.NY/T 788—2004.农药残留试验准则[S].北京:中国标准出版社,2004.
[13]韦婕,宋世明,李雪生.高效液相色谱法检测番茄中乙撑硫脲和丙撑硫脲的残留[J].农药,2016,55(12):912-914.
[14]刘亚娟,侯志广,梁爽,等.70%扑草净·乙草胺SE在花生中的残留分析方法[J].农药,2017,56(3):193-196.
[2]杨吉春,王秀丽,杨帆.2013年公开的新农药品种[J].农药,2014,53(2):123-125.
[3]RATTAN R S,SINGH V,PAN Y F,et al.Du PontTM PyraxaltTM(DPX-RAB55;Triflumezopyrim):Low Sensitivity to Natural Enemies of Rice Ecosystem[C]//International Iupac Conference on“Agrochemicals Protecting Crop,Health and Natural Environment New Chemistries for Phytomedicines and Crop Protection Chemicals.2016:61.
[4]杨光.杜邦三氟苯嘧啶将获我国首登[J].农药市场信息,2016(8):606.
[5]JR H C,CORDOVA D,ZHANG Wen-ming,et al.Mesoionic Insecticides:A Novel Class of Insecticides that Modulate Nicotinic Acetylcholine Receptors[J].Pest Management Science,2017,73(4):796-806.
[6]CORDOVA D,BENNER E A,SCHROEDER M E,et al.Mode of Action of Triflumezopyrim:A Novel Mesoionic Insecticide Which Inhibits the Nicotinic Acetylcholine Receptor[J].Insect Biochemistry&Molecular Biology,2016(74):32.
[7]ZHANG Wen-ming,JR C W H,PAHUTSKI T F,et al.Mesoionic Pyrido[1,2-a]Pyrimidinones:Discovery of Triflumezopyrim as a Potent Hopper Insecticide 1[J].Bioorganic&Medicinal Chemistry Letters,2017,27(1):16-20.
[8]SINGH V,TEIXEIRA L,VINCENT D,et al.Triflumezopyrim(Pyraxalt TM)-A New Approach to Rice Plant Hopper Management in Asia Pacific[C]//Xxv International Congress of Entomology.2016.
[9]唐涛,叶波,刘雪源,等.多靶标杀虫剂—三氟苯嘧啶混配剂对水稻害虫的田间防治效果[J].植物保护,2016,42(6):202-207.
[10]SINGH V,TEIXEIRA L,LEIGHTY R M,et al.Du PontTM PyraxaltTM(DPX-RAB55;Triflumezopyrim):A novel chemistry for Rice Planthopper Management in Asia Pacific[C]//International Iupac Conference on“Agrochemicals Protecting Crop,Health and Natural Environment New Chemistries for Phytomedicines and Crop Protection Chemicals.2016.
[11]俞建忠,谢昀,姜宜飞,等.Triflumezopyrim 10%悬浮剂高效液相色谱分析方法研究[J].农药科学与管理,2015,36(3):49-51.
[12]中华人民共和国农业部.NY/T 788—2004.农药残留试验准则[S].北京:中国标准出版社,2004.
[13]韦婕,宋世明,李雪生.高效液相色谱法检测番茄中乙撑硫脲和丙撑硫脲的残留[J].农药,2016,55(12):912-914.
[14]刘亚娟,侯志广,梁爽,等.70%扑草净·乙草胺SE在花生中的残留分析方法[J].农药,2017,56(3):193-196.