一种20%氯虫苯甲酰胺悬浮剂的液相色谱检测方法研究
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摘要
为研究筛选出一种高效液相色谱技术检测20%氯虫苯甲酰胺悬浮剂的最佳方法,首先通过液相色谱检测不同浓度的标准品建立标准曲线(y=2.9×105x-1.8×106,R2=0.9999),然后通过对5种不同提取剂(甲醇、乙醇、乙腈、苯酮、二氯甲烷)的提取样品后液相色谱结果进行比较研究,筛选出其中较好的提取试剂-二氯甲烷,并且其最佳浓度为55%(20%氯虫苯甲酰胺悬浮剂-康宽的检出浓度为931.4μg/m L)。研究建立了一种氯虫苯甲酰胺最佳液相色谱方法(在常规的液相色谱条件下,以55%的二氯甲烷提取),为氯虫苯甲酰胺后续的残留以及消解等方面研究提供了参考。
This paper aims to find the best way to detect 20% chlorantraniliprole suspension liquid by usinghigh performance liquid chromatography(HPLC). Firstly, the standard curve was built through detectingdifferent dosages of the standard sample method by HPLC. Secondly, the research showed that HPLC result ofdichloromethane was the best among 5 different extracting materials(solvent methanol, ethanol, acetonitrile,acetone and dichloromethane) and the best dosage for extracting was 55%. It was found that the best HPLC wayfor detecting 20% chlorantraniliprole suspension liquid was using 55% dichloromethane to extract thechlorantraniliprole(detectable concentration of 20% chlorantraniliprole SC- CORAGEN was 931.4 μg/m L).The research established the best HPLC way to detect chlorantraniliprole and could provide references forfurther study on the residue and elimination of chlorantraniliprole.
This paper aims to find the best way to detect 20% chlorantraniliprole suspension liquid by usinghigh performance liquid chromatography(HPLC). Firstly, the standard curve was built through detectingdifferent dosages of the standard sample method by HPLC. Secondly, the research showed that HPLC result ofdichloromethane was the best among 5 different extracting materials(solvent methanol, ethanol, acetonitrile,acetone and dichloromethane) and the best dosage for extracting was 55%. It was found that the best HPLC wayfor detecting 20% chlorantraniliprole suspension liquid was using 55% dichloromethane to extract thechlorantraniliprole(detectable concentration of 20% chlorantraniliprole SC- CORAGEN was 931.4 μg/m L).The research established the best HPLC way to detect chlorantraniliprole and could provide references forfurther study on the residue and elimination of chlorantraniliprole.
引文
[1]柴宝山,林丹,刘远雄,等.新型邻甲酰氨基苯甲酰胺类杀虫剂的研究进展[J].农药,2007,46(3):148-153.
[2]吴永果,毛春晖,兰支利.3-溴-1-(3-氯-2-吡啶基)-4,5-二氢-1H-吡唑-5-甲酸乙酯的合成研究[J].精细化工中间体,2007,37(5):15-17.
[3]Tomlin C.The pesticide manual[M].Brighton:The British Crop Protection Council,2006:1022.
[4]Bassi A,Alber R.Chlorantraniliprole:a novel anthranilic diamide insecticide[C].IAPPS.X V I International Plant Protection Congress,Glasgrow UK:BCPC,2007:52-59.
[5]闫潇敏,宁斌科,王列平,等.新型邻酰胺基苯甲酰胺类杀虫剂氯虫苯甲酰胺的合成与应用[J].世界农药,2009,12:20-23.
[6]刘芳,奚本贵,包善微,等.氯虫苯甲酰胺对稻纵卷叶螟的防效及对稻田有益节肢动物的安全性评价[J].植物保护,2009,35(5):139-143.
[7]徐广春,顾中言,徐德进,等.氯虫苯甲酰胺和噻虫胺对水稻的表观安全性评价[J].农药,2009,48(10):752-754.
[8]Lahm G P,Selby T P,Freudenberger J H,et al.Insecticidal anthranilic diamides:a new class of potent ryanodine receptor activators[J].Bioorganic and Medicinal Chemistry Letters,2005,15(22):4898-4906.
[9]Lahm G P,Stevenson T M,Selby T P,et al.a new insecticidal anthranilic diamide that acts as a potent and selective ryanodine receptor activator[J].Bioorganic and Medicinal Chemistry Letters,2007,17(22):6274-6279.
[10]Liu G Y,Ju X L,Cheng J,Liu Z Q.3D-QSAR studies of insecticidal anthranilic diamides as ryanodine receptor activators using Co MFA,Co MSIA and DISCOtech[J].Chemosphere,2010,78:300-306.
[11]Sattelle D B,Cordova D,Cheek T R.Insect ryanodine receptors:molecular targets for novel pest control chemicals[J].Invertebrate Neuroscience,2008,8:107-119.
[12]柴宝山,林丹,刘远雄,等.新型邻甲酰氨基苯甲酰胺类杀虫剂的研究进展[J].农药,2007,46(3):148-153.
[13]董波,孙国俊,蒋林忠,等.茚虫威15%乳油和氯虫苯甲酰胺20%悬浮剂对稻纵卷叶螟的防效试验[J].农药科学与管理,2009,30(3):31-32,44.
[14]张武军,张辉,张伟,等.18.5%氯虫苯甲酰胺悬浮剂防治水稻二化螟药效试验[J].农药,2009,48(3):230-232.
[15]Cao G C,Lu Q,Zhang L L,et al.Toxicity of chlorantraniliprole to Cry1Ac-susceptible and resistant strains of Helicoverpa armigera[J].Pesticide Biochemistry and Physiology,2010,98(1):99-103.
[16]徐妍,战瑞,马超,等.30%噻虫嗪·氯虫苯甲酰胺悬浮剂高效液相色谱分析[J].农药,2009,48(7):494-495,503.
[17]王广成,吴春先,高立明,等.氯虫苯甲酰胺悬浮剂的高效液相色谱分析[J].农药,2009,48(4):267-269.
[18]陈小军,费春,樊丽萍,等.氯虫苯甲酰胺在大豆植株中的内吸传导特性[J].中国农业科学,2011,44(11):2276-2283.
[19]Caboni P,Sarais G,Angioni A,et al.Liquid chromatographytandem mass spectrometric ion-switching determination of chlorantraniliprole and flubendiamide in fruits and vegetables[J].Journal of Agricultural and Food Chemistry,2008,56(17):7696-7699.
[20]Grant J,Rodgers C A,Chickering C D,et al.Determination of chlorantraniliprole residues in crops by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry/mass spectrometry[J].Journal of AOAC International,2010,93(4):1293-1301.
[21]步海燕,欧晓明,马俊凯,等.高效液相色谱法测定水体中的氯虫苯甲酰胺残留量[J].光谱实验室,2008,25(6):1230-1234.
[22]秦冬梅,秦旭,徐应明,等.土壤和番茄中氯虫苯甲酰胺的残留检测与消解动态研究[J].农业环境科学学报,2010,29(5):858-863.
[23]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.
[24]李岩,于荣,吴进龙,等.氯苯·高氯氟150 g/L微囊悬浮-悬浮剂液相色谱分析方法研究[J].农药科学与管理,2009,30(8):38-41.
[25]张云,郑敬峰,李耀平,等.液相色谱-串联质谱测定动物源性食品中氯虫苯甲酰胺和氯虫酰胺残留量[J].食品科学.2013,34(10):272-275.
[26]崔荣海,宋建华,姜义平,等.高效液相色谱法分析水中氯虫苯甲酰胺[J].广东农业科学,2012,17:103-105.
[2]吴永果,毛春晖,兰支利.3-溴-1-(3-氯-2-吡啶基)-4,5-二氢-1H-吡唑-5-甲酸乙酯的合成研究[J].精细化工中间体,2007,37(5):15-17.
[3]Tomlin C.The pesticide manual[M].Brighton:The British Crop Protection Council,2006:1022.
[4]Bassi A,Alber R.Chlorantraniliprole:a novel anthranilic diamide insecticide[C].IAPPS.X V I International Plant Protection Congress,Glasgrow UK:BCPC,2007:52-59.
[5]闫潇敏,宁斌科,王列平,等.新型邻酰胺基苯甲酰胺类杀虫剂氯虫苯甲酰胺的合成与应用[J].世界农药,2009,12:20-23.
[6]刘芳,奚本贵,包善微,等.氯虫苯甲酰胺对稻纵卷叶螟的防效及对稻田有益节肢动物的安全性评价[J].植物保护,2009,35(5):139-143.
[7]徐广春,顾中言,徐德进,等.氯虫苯甲酰胺和噻虫胺对水稻的表观安全性评价[J].农药,2009,48(10):752-754.
[8]Lahm G P,Selby T P,Freudenberger J H,et al.Insecticidal anthranilic diamides:a new class of potent ryanodine receptor activators[J].Bioorganic and Medicinal Chemistry Letters,2005,15(22):4898-4906.
[9]Lahm G P,Stevenson T M,Selby T P,et al.a new insecticidal anthranilic diamide that acts as a potent and selective ryanodine receptor activator[J].Bioorganic and Medicinal Chemistry Letters,2007,17(22):6274-6279.
[10]Liu G Y,Ju X L,Cheng J,Liu Z Q.3D-QSAR studies of insecticidal anthranilic diamides as ryanodine receptor activators using Co MFA,Co MSIA and DISCOtech[J].Chemosphere,2010,78:300-306.
[11]Sattelle D B,Cordova D,Cheek T R.Insect ryanodine receptors:molecular targets for novel pest control chemicals[J].Invertebrate Neuroscience,2008,8:107-119.
[12]柴宝山,林丹,刘远雄,等.新型邻甲酰氨基苯甲酰胺类杀虫剂的研究进展[J].农药,2007,46(3):148-153.
[13]董波,孙国俊,蒋林忠,等.茚虫威15%乳油和氯虫苯甲酰胺20%悬浮剂对稻纵卷叶螟的防效试验[J].农药科学与管理,2009,30(3):31-32,44.
[14]张武军,张辉,张伟,等.18.5%氯虫苯甲酰胺悬浮剂防治水稻二化螟药效试验[J].农药,2009,48(3):230-232.
[15]Cao G C,Lu Q,Zhang L L,et al.Toxicity of chlorantraniliprole to Cry1Ac-susceptible and resistant strains of Helicoverpa armigera[J].Pesticide Biochemistry and Physiology,2010,98(1):99-103.
[16]徐妍,战瑞,马超,等.30%噻虫嗪·氯虫苯甲酰胺悬浮剂高效液相色谱分析[J].农药,2009,48(7):494-495,503.
[17]王广成,吴春先,高立明,等.氯虫苯甲酰胺悬浮剂的高效液相色谱分析[J].农药,2009,48(4):267-269.
[18]陈小军,费春,樊丽萍,等.氯虫苯甲酰胺在大豆植株中的内吸传导特性[J].中国农业科学,2011,44(11):2276-2283.
[19]Caboni P,Sarais G,Angioni A,et al.Liquid chromatographytandem mass spectrometric ion-switching determination of chlorantraniliprole and flubendiamide in fruits and vegetables[J].Journal of Agricultural and Food Chemistry,2008,56(17):7696-7699.
[20]Grant J,Rodgers C A,Chickering C D,et al.Determination of chlorantraniliprole residues in crops by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry/mass spectrometry[J].Journal of AOAC International,2010,93(4):1293-1301.
[21]步海燕,欧晓明,马俊凯,等.高效液相色谱法测定水体中的氯虫苯甲酰胺残留量[J].光谱实验室,2008,25(6):1230-1234.
[22]秦冬梅,秦旭,徐应明,等.土壤和番茄中氯虫苯甲酰胺的残留检测与消解动态研究[J].农业环境科学学报,2010,29(5):858-863.
[23]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.
[24]李岩,于荣,吴进龙,等.氯苯·高氯氟150 g/L微囊悬浮-悬浮剂液相色谱分析方法研究[J].农药科学与管理,2009,30(8):38-41.
[25]张云,郑敬峰,李耀平,等.液相色谱-串联质谱测定动物源性食品中氯虫苯甲酰胺和氯虫酰胺残留量[J].食品科学.2013,34(10):272-275.
[26]崔荣海,宋建华,姜义平,等.高效液相色谱法分析水中氯虫苯甲酰胺[J].广东农业科学,2012,17:103-105.