三气相色谱-三重四级杆质谱法同时测定农药中32种隐性添加成分
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摘要
目的建立气相色谱-三重四级杆质谱法(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)对农药制剂中32种隐性添加农药成分的分析方法。方法样品采用丙酮直接提取,正己烷定容,内标法定量,气相色谱-串联质谱仪检测。结果 32种农药的平均添加回收率为71.51%~100.88%,相对标准偏差(relative standard deviation,RSD)为1.36%~7.43%,检出限为0.03%~0.17%,定量限为0.1%~0.5%。采用建立的方法对抽检的农药产品进行检测,结果表明部分农药中检出隐性成分,在0.5%的苦参碱水剂中检出1.6%的氰戊菊酯,在5%的高效氯氟氰菊酯中检出3.5%的氟虫腈。结论该方法高效、准确,可用于同时测定农药中的32种隐性添加农药成分。
Objective To establish a method for determination of 32 kinds of implicitly added ingredients in pesticide formulations by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).Methods The samples were directly extracted with acetone,and volumed with n-hexane.Then they were detected by GC-MS/MS and quantified by internal standard method.Results The average recoveries of 32 kinds of pesticides were 71.51%-100.88% and the relative standard deviations(RSDs) were 1.36%-7.43%.The limits of detection were 0.03%-0.17%,and the limits of quantification were 0.1%-0.5%.The established method was used to detect pesticide products,and the results showed that some of the pesticides were detected in recessive ingredients.Totally 1.6% of fenvalerate was detected in 0.5% of matrine aqueous solution,and 3.5% of fipronil was detected in 5% of lambda-cyhalothrin.Conclusion The method is efficient and accurate,which can be used for simultaneous determination of 32 kinds of implicitly added ingredients in pesticides.
Objective To establish a method for determination of 32 kinds of implicitly added ingredients in pesticide formulations by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).Methods The samples were directly extracted with acetone,and volumed with n-hexane.Then they were detected by GC-MS/MS and quantified by internal standard method.Results The average recoveries of 32 kinds of pesticides were 71.51%-100.88% and the relative standard deviations(RSDs) were 1.36%-7.43%.The limits of detection were 0.03%-0.17%,and the limits of quantification were 0.1%-0.5%.The established method was used to detect pesticide products,and the results showed that some of the pesticides were detected in recessive ingredients.Totally 1.6% of fenvalerate was detected in 0.5% of matrine aqueous solution,and 3.5% of fipronil was detected in 5% of lambda-cyhalothrin.Conclusion The method is efficient and accurate,which can be used for simultaneous determination of 32 kinds of implicitly added ingredients in pesticides.
引文
[1]李俊,赵为武,郭晓关,等.乳油型农药中多种禁止使用农药成分的同时检测[J].农药,2012,51(1):44-46.Li J,Zhao WW,Guo XG,et al.Simultaneous determination method for forbidden pesticide composition in EC[J].Agrochemical,2012,51(1):44-46.
[2]束放,熊延坤.我国农药生产现状和农药减量使用的重要意义[J].山东农药信息,2016,(2):18-20.Su F,Xiong YK.The current situation of pesticide production and the significance of the use of pesticide reduction in China[J].Shandong Pest Inf,2016,(2):18-20.
[3]段又生.数据分析我国农药行业发展态势[J].中国农药,2016,(1):46-55.Duan YS.Data analysis of the pesticide industry in China[J].Chin Pest,2016,(1):46-55.
[4]郭映花,杨惠芳.我国禁(限)用农药的管理与控制现状[J].现代预防医学,2013,40(12):2198-2202.Guo YH,Yang HF.The management and control status of banned/restricted pesticides in China[J].Mod Prev Med,2013,40(12):2198-2202.
[5]乔成奎,黄玉南,罗静,等.HPLC-MS/MS法检测农药产品中30种隐性成分[J].农药,2015,54(5):340-342,345.Qiao CK,Huang YN,Luo J,et al.Determination of 30 hidden ingredients in pesticide products by HPLC-MS/MS[J].Agrochemical,2015,54(5):340-342,345.
[6]陆小磊,蒋美蓉,叶美君,等.固相萃取净化-气相色谱质谱法测定茶叶中22种禁用农药残留量[J].中国茶叶加工,2015(1):11-17.Lu XL,Jiang MR,Ye MJ,et al.Determination of 22 banned pesticides residues in tea by solid phase extraction and gas chromatography mass spectrometry[J].China Tea Process,2015(1):11-17.
[7]陈晓明,王程龙,薄瑞.中国农药使用现状及对策建议[J].农药科学与管理,2016,37(2):4-8.Chen XM,Wang CL,Bo R,et al.Current situation of Chinese pesticide application and policy suggestions[J].Pest Sci Admin,2016,37(2):4-8.
[8]Zhou P,Lu YT,Liu BF,et al.Dynamics of fipronil residue in vegetable-field ecosystem[J].Chemosphere,2004,57(11):1691-1696.
[9]Yi XH,Lu YT.Residues and dynamics of probenazole in rice field ecosystem[J].Chemosphere,2006,65(4):639-643.
[10]袁善奎,刘亮,王以燕,等.农药非法添加隐性成分及其风险分析[J].农药,2016,55(7):480-482,490.Yuan SK,Liu L,Wang YY,et al.Illegal addition of pesticides to hidden ingredients and its risk analysis[J].Agrochemical,2016,55(7):480-482,490.
[11]张寒,黄晓华,徐永.农药隐性成分现状分析及对策[J].农药科学与管理,2017,38(5):6-10,20.Zhang H,Huang XH,Xu Y.Situation of hidden ingredients in pesticides analysis and countermeasures[J].Pest Sci Admin,2017,38(5):6-10,20.
[12]包素萍,张晓强,武中平,等.HPLC-MS联用技术同时检测12种杀虫剂[J].农药,2014,53(4):257-259.Bao SP,Zhang XQ,Wu ZP,et al.HPLC-MS technique for the simultaneous detection of 12 pesticides[J].Agrochemical,2014,53(4):257-259.
[13]孙长恩,洪华,潘虹,等.化学杀虫剂中9种拟除虫菊酯检测方法[J].江苏农业科学,2014,42(4):273-275.Sun CE,Hong H,Pan H,et al.Determination of 9 pyrethroids in chemical insecticides[J].Jiangsu Agric Sci,2014,42(4):273-275.
[14]吴升德,胡天良,蔡云,等.气相色谱法分析杀虫气雾剂中5种拟除虫菊酯类农药[J].农药,2015,54(3):191-193.Wu SD,Hu TL,Cai Y,et al.Analysis of five pyrethroid pesticides in insecticide aerosols by gas chromatography[J].Agrochemical,2015,54(3):191-193.
[15]洪华,张晓强,武中平,等.SPE-GC-MS快速定性定量杀虫剂产品中11种违禁添加菊酯类隐性成分[J].农药,2013,52(11):812-814.Hong H,Zhang XQ,Wu ZP,et al.SPE-GC-MS rapid qualitative and quantitative 11 kinds of banned add pyrethroid stealth component in pesticides products[J].Agrochemical,2013,52(11):812-814.
[2]束放,熊延坤.我国农药生产现状和农药减量使用的重要意义[J].山东农药信息,2016,(2):18-20.Su F,Xiong YK.The current situation of pesticide production and the significance of the use of pesticide reduction in China[J].Shandong Pest Inf,2016,(2):18-20.
[3]段又生.数据分析我国农药行业发展态势[J].中国农药,2016,(1):46-55.Duan YS.Data analysis of the pesticide industry in China[J].Chin Pest,2016,(1):46-55.
[4]郭映花,杨惠芳.我国禁(限)用农药的管理与控制现状[J].现代预防医学,2013,40(12):2198-2202.Guo YH,Yang HF.The management and control status of banned/restricted pesticides in China[J].Mod Prev Med,2013,40(12):2198-2202.
[5]乔成奎,黄玉南,罗静,等.HPLC-MS/MS法检测农药产品中30种隐性成分[J].农药,2015,54(5):340-342,345.Qiao CK,Huang YN,Luo J,et al.Determination of 30 hidden ingredients in pesticide products by HPLC-MS/MS[J].Agrochemical,2015,54(5):340-342,345.
[6]陆小磊,蒋美蓉,叶美君,等.固相萃取净化-气相色谱质谱法测定茶叶中22种禁用农药残留量[J].中国茶叶加工,2015(1):11-17.Lu XL,Jiang MR,Ye MJ,et al.Determination of 22 banned pesticides residues in tea by solid phase extraction and gas chromatography mass spectrometry[J].China Tea Process,2015(1):11-17.
[7]陈晓明,王程龙,薄瑞.中国农药使用现状及对策建议[J].农药科学与管理,2016,37(2):4-8.Chen XM,Wang CL,Bo R,et al.Current situation of Chinese pesticide application and policy suggestions[J].Pest Sci Admin,2016,37(2):4-8.
[8]Zhou P,Lu YT,Liu BF,et al.Dynamics of fipronil residue in vegetable-field ecosystem[J].Chemosphere,2004,57(11):1691-1696.
[9]Yi XH,Lu YT.Residues and dynamics of probenazole in rice field ecosystem[J].Chemosphere,2006,65(4):639-643.
[10]袁善奎,刘亮,王以燕,等.农药非法添加隐性成分及其风险分析[J].农药,2016,55(7):480-482,490.Yuan SK,Liu L,Wang YY,et al.Illegal addition of pesticides to hidden ingredients and its risk analysis[J].Agrochemical,2016,55(7):480-482,490.
[11]张寒,黄晓华,徐永.农药隐性成分现状分析及对策[J].农药科学与管理,2017,38(5):6-10,20.Zhang H,Huang XH,Xu Y.Situation of hidden ingredients in pesticides analysis and countermeasures[J].Pest Sci Admin,2017,38(5):6-10,20.
[12]包素萍,张晓强,武中平,等.HPLC-MS联用技术同时检测12种杀虫剂[J].农药,2014,53(4):257-259.Bao SP,Zhang XQ,Wu ZP,et al.HPLC-MS technique for the simultaneous detection of 12 pesticides[J].Agrochemical,2014,53(4):257-259.
[13]孙长恩,洪华,潘虹,等.化学杀虫剂中9种拟除虫菊酯检测方法[J].江苏农业科学,2014,42(4):273-275.Sun CE,Hong H,Pan H,et al.Determination of 9 pyrethroids in chemical insecticides[J].Jiangsu Agric Sci,2014,42(4):273-275.
[14]吴升德,胡天良,蔡云,等.气相色谱法分析杀虫气雾剂中5种拟除虫菊酯类农药[J].农药,2015,54(3):191-193.Wu SD,Hu TL,Cai Y,et al.Analysis of five pyrethroid pesticides in insecticide aerosols by gas chromatography[J].Agrochemical,2015,54(3):191-193.
[15]洪华,张晓强,武中平,等.SPE-GC-MS快速定性定量杀虫剂产品中11种违禁添加菊酯类隐性成分[J].农药,2013,52(11):812-814.Hong H,Zhang XQ,Wu ZP,et al.SPE-GC-MS rapid qualitative and quantitative 11 kinds of banned add pyrethroid stealth component in pesticides products[J].Agrochemical,2013,52(11):812-814.