植物油中邻氨基苯甲二酰胺类农药残留检测技术研究
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摘要
建立了同时测定植物油中溴氰虫酰胺、氟虫双酰胺、氯虫苯甲酰胺3种邻氨基苯甲二酰胺类农药残留的凝胶渗透色谱(GPC)-液相色谱检测方法。植物油中残留的邻氨基苯甲二酰胺类农药,经环已烷-乙酸乙酯混合溶液提取后,用凝胶渗透色谱系统净化,以乙腈∶0.1mol/L的乙酸铵水溶液(58∶42)作为流动相,DAD检测器测定,外标法定量。测定结果表明:采用本方法检测植物油中3种邻氨基苯甲二酰胺类农药,方法检出限均能达到0.1mg/kg,在标准曲线质量浓度0.1~2 mg/L之间线性相关系数均大于0.999 8,在0.1、0.2、1mg/kg水平添加回收,回收率在70.1%~99.1%范围之间,准确度较高;相对标准偏差范围在3.0%~9.7%之间,精密度较好。
A gel permeation chromatography( GPC)-liquid chromatography method was developed for the simultaneous determination of 3 kinds of o-amino benzoic diamide pesticide residues( cyantraniliprole,flubendiamide and chlorantraniliprole) in vegetable oil. O-amino benzoic diamide pesticide residues in vegetable oil extracted with cyclohexane and ethyl acetate mixture solution was purified by gel permeation chromatography system; acetonitrile and0. 1 mol/L ammonium acetate aqueous solution( 58∶ 42) was taken as mobile phase to determine by the DAD detector and quantify by external standard method. The results showed that by using this method to determine 3 kinds of o-amino benzoic diamide pesticides,the limit of detection could achieved 0. 1 mg/kg; the relative modular were better than 0. 9998 for the standard curve concentration between 0. 1 ~ 2 mg/L; the recoveries were between 70. 1% ~99. 1% for 0. 1,0. 2,1 mg/kg add level; the relatively standard deviations( RSDs) were between 3. 0% ~ 9. 7%with a good degree of precision.
A gel permeation chromatography( GPC)-liquid chromatography method was developed for the simultaneous determination of 3 kinds of o-amino benzoic diamide pesticide residues( cyantraniliprole,flubendiamide and chlorantraniliprole) in vegetable oil. O-amino benzoic diamide pesticide residues in vegetable oil extracted with cyclohexane and ethyl acetate mixture solution was purified by gel permeation chromatography system; acetonitrile and0. 1 mol/L ammonium acetate aqueous solution( 58∶ 42) was taken as mobile phase to determine by the DAD detector and quantify by external standard method. The results showed that by using this method to determine 3 kinds of o-amino benzoic diamide pesticides,the limit of detection could achieved 0. 1 mg/kg; the relative modular were better than 0. 9998 for the standard curve concentration between 0. 1 ~ 2 mg/L; the recoveries were between 70. 1% ~99. 1% for 0. 1,0. 2,1 mg/kg add level; the relatively standard deviations( RSDs) were between 3. 0% ~ 9. 7%with a good degree of precision.
引文
[1]李娜.食用油安全问题浅析[J].中国粮食经济,2008,(3):17-18Li Na.Analysis on the safety of edible oil[J].China Grain Economy,2008,(3):17-18
[2]徐尚成,俞幼芬,王晓军,等.新杀虫剂氯虫苯甲酰胺及其研究开发进展[J].现代农药,2008,7(5):8-11Xu Shangcheng,Yu Youfen,Wang Xiaojun,et al.Rynaxypyr,a new insecticide and its research&development in application[J].Modern Agrochemicals,2008,7(5):8-11
[3]Caballero R,Cyman S,Schuster D J,et al,Baseline susceptibility of Bemisia tabaci(Genn.)biotype B in southern Florida to cyantraniliprole[J].Crop Protection,2013,44:104-108
[4]Lahm G P,Cordova D,Barry J D.New and selective ryanodine receptor a ctivators for insect control[J].Bioorganic&Medicinal Chemistry,2009,17(3):4127-4133
[5]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):148-153Chai Baoshan,Lin Dan,Liu Yuanxiong,et al.Recent advance on novel insecticidal anthranilic diamides[J].Pesticides,2007,46(3):148-153
[6]DUPONT.Rynaxypyr Technical Bulletin[R].2007-12-27
[7]US EPA.Frdrral Register,2007,72(94):27452-27456
[8]Codex Alimentarius Commission.Pesticide residues in food and feed[DB/OL]
[9]European Commission.EU pesticides database[DB/OL]
[10]United States Department of Agriculture.Maximum residue Limits(MRL)database[DB/OL]
[11]The Japan Food Chemical Research Foundation.The Japanese positive list system for agricultural chemical residues in foods[DB/OL]
[12]GB/T 2763-2014食品安全国家标准食品中农药最大残留量[S]GB/T 2763-2014 National food safety standard Maximum residue limits for pesticides in food[S]
[13]亢晓冬,孙霞,沈礼,等.氯虫苯甲酰胺的高效液相色谱分析方法研究[J].浙江化工,2010,41(4):31-32Kang Xiaodong,Sun Xia,Shen Li,et al.Analysis of chlorantraniliprole by HPLC[J].Zhejiang Chemical Industry,2010,41(4):31-32
[14]张云,李今中,李耀平,等.液相色谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量[J].分析试验室,2012,31(4),119-122Zhang Yun,Li Jinzhong,Li Yaoping,et al.Determination chloranteraniliprole and flubendiamide residues in foodstuffs of animal origin by high performance liquid chromatography[J].Chinese Journal of Analysis Laboratory,2012,31(4),119-122
[15]张云,郑敬峰,李耀平,等.液相色谱-串联质谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量[J].食品科学,2013,34(10),272-275Zhang Yun,Zheng Jingfeng,Li Yaoping,et al.LC-MS/MS determination of chloranteraniliprole and flubendiamide residues in animal-derived foodstuffs[J].Food Science,2013,34(10),272-275
[16]郭岚,谢明勇,鄢爱平,等.GPC-GC-MS对食用植物油中多种类型农药残留的同步测定[J].分析测试学报,2009,28(1):67-71Guo Lan,Xie Mingyong,Yan Aiping,et al.Simultaneous determination of multi-types of pesticide residues in edible vegetable oils by GPC-GC-MS method[J].Journal of Instrumental Analysis,2009,28(1):67-71
[17]黎其万,刘宏程.测定植物油中甲奈威和克百威农药残留的高效液相色谱法[J].食品与发酵工业,2005,8:91-92Li Qiwan,Liu Hongcheng.Determination of vegetable oil in a Budweiser Neville and grams of pesticide residues in chromatography[J].Food and Fermentation Industries,2005,8:91-92
[18]吴丽华.固相萃取-气相色谱法测定植物油中多种拟虫菊酯类农药残留的方法探讨[J].粮食与粮食工业,2013(2):62-67Wu Lihua.A method for the determination of several kinds of pesticide residues in vegetable oils by gas chromatography with solid phase extraction and gas chromatography to study the[J].grain and grain industry,2013(2):62-67
[19]阮华,荣维广,宋宁慧,等.Qu ECh ERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留[J].分析化学,2014,42(8):1110-1116Ruan Hua,Rong Weiguang,Song Ninghui,et al.Simultaneous determination of 34 pesticide residues in vegetable oil by Qu ECh ERS-on-line gel permeation chromatography-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(8):1110-1116
[20]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):38-41Li Yan,Yu Rong,Wu Jinlong,et al.Analytical method for Lambda-cyhalothrin.Chlorantraniliprole 150g/L ZC by HPLC[J].Pesticide Science and Administration,2009,30(8):38-41.
[2]徐尚成,俞幼芬,王晓军,等.新杀虫剂氯虫苯甲酰胺及其研究开发进展[J].现代农药,2008,7(5):8-11Xu Shangcheng,Yu Youfen,Wang Xiaojun,et al.Rynaxypyr,a new insecticide and its research&development in application[J].Modern Agrochemicals,2008,7(5):8-11
[3]Caballero R,Cyman S,Schuster D J,et al,Baseline susceptibility of Bemisia tabaci(Genn.)biotype B in southern Florida to cyantraniliprole[J].Crop Protection,2013,44:104-108
[4]Lahm G P,Cordova D,Barry J D.New and selective ryanodine receptor a ctivators for insect control[J].Bioorganic&Medicinal Chemistry,2009,17(3):4127-4133
[5]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):148-153Chai Baoshan,Lin Dan,Liu Yuanxiong,et al.Recent advance on novel insecticidal anthranilic diamides[J].Pesticides,2007,46(3):148-153
[6]DUPONT.Rynaxypyr Technical Bulletin[R].2007-12-27
[7]US EPA.Frdrral Register,2007,72(94):27452-27456
[8]Codex Alimentarius Commission.Pesticide residues in food and feed[DB/OL]
[9]European Commission.EU pesticides database[DB/OL]
[10]United States Department of Agriculture.Maximum residue Limits(MRL)database[DB/OL]
[11]The Japan Food Chemical Research Foundation.The Japanese positive list system for agricultural chemical residues in foods[DB/OL]
[12]GB/T 2763-2014食品安全国家标准食品中农药最大残留量[S]GB/T 2763-2014 National food safety standard Maximum residue limits for pesticides in food[S]
[13]亢晓冬,孙霞,沈礼,等.氯虫苯甲酰胺的高效液相色谱分析方法研究[J].浙江化工,2010,41(4):31-32Kang Xiaodong,Sun Xia,Shen Li,et al.Analysis of chlorantraniliprole by HPLC[J].Zhejiang Chemical Industry,2010,41(4):31-32
[14]张云,李今中,李耀平,等.液相色谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量[J].分析试验室,2012,31(4),119-122Zhang Yun,Li Jinzhong,Li Yaoping,et al.Determination chloranteraniliprole and flubendiamide residues in foodstuffs of animal origin by high performance liquid chromatography[J].Chinese Journal of Analysis Laboratory,2012,31(4),119-122
[15]张云,郑敬峰,李耀平,等.液相色谱-串联质谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量[J].食品科学,2013,34(10),272-275Zhang Yun,Zheng Jingfeng,Li Yaoping,et al.LC-MS/MS determination of chloranteraniliprole and flubendiamide residues in animal-derived foodstuffs[J].Food Science,2013,34(10),272-275
[16]郭岚,谢明勇,鄢爱平,等.GPC-GC-MS对食用植物油中多种类型农药残留的同步测定[J].分析测试学报,2009,28(1):67-71Guo Lan,Xie Mingyong,Yan Aiping,et al.Simultaneous determination of multi-types of pesticide residues in edible vegetable oils by GPC-GC-MS method[J].Journal of Instrumental Analysis,2009,28(1):67-71
[17]黎其万,刘宏程.测定植物油中甲奈威和克百威农药残留的高效液相色谱法[J].食品与发酵工业,2005,8:91-92Li Qiwan,Liu Hongcheng.Determination of vegetable oil in a Budweiser Neville and grams of pesticide residues in chromatography[J].Food and Fermentation Industries,2005,8:91-92
[18]吴丽华.固相萃取-气相色谱法测定植物油中多种拟虫菊酯类农药残留的方法探讨[J].粮食与粮食工业,2013(2):62-67Wu Lihua.A method for the determination of several kinds of pesticide residues in vegetable oils by gas chromatography with solid phase extraction and gas chromatography to study the[J].grain and grain industry,2013(2):62-67
[19]阮华,荣维广,宋宁慧,等.Qu ECh ERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留[J].分析化学,2014,42(8):1110-1116Ruan Hua,Rong Weiguang,Song Ninghui,et al.Simultaneous determination of 34 pesticide residues in vegetable oil by Qu ECh ERS-on-line gel permeation chromatography-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(8):1110-1116
[20]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):38-41Li Yan,Yu Rong,Wu Jinlong,et al.Analytical method for Lambda-cyhalothrin.Chlorantraniliprole 150g/L ZC by HPLC[J].Pesticide Science and Administration,2009,30(8):38-41.