分散固相萃取-液相色谱质谱法测定多种基质中的氰氟草酯和氰氟草酸
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摘要
建立了田水、土壤、水稻植株、水稻稻壳和糙米中氰氟草酯及代谢产物氰氟草酸的残留分析方法。前处理方法利用乙腈为提取剂,N-丙基乙二胺(PSA)、石墨化碳黑(GCB)和C18为分散净化剂的QuEChERS方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式(MRN)下进行检测,外标法定量。结果表明:氰氟草酯和氰氟草酸在0. 01～1. 0 mg·L~(-1)浓度范围内均具有良好的线性关系(R~2≥0. 997);在0. 05～1. 00 mg·kg~(-1)添加水平范围内平均回收率为70. 6%～105. 8%;相对标准偏差(RSD,n=5)为0. 3%～7. 9%;氰氟草酯和氰氟草酸的方法检出限(LOD)为0. 11和0. 16μg·kg~(-1);定量限为0. 37和0. 54μg·kg~(-1)。该方法分析速度快、灵敏度高、重现性好,适用于多种基质上氰氟草酯和氰氟草酸的快速检测和确证。
A method was developed for the simultaneous determination of cyhalofop-butyl and cyhalofop-caid in rice plant,rice,rice hull,paddyfield water and paddyfield soil.The residues were extracted from samples with acetonitrile and cleaned up with dispersive method on PSA,GCB and C18,then detected by ultra liquidchromatography-mass spectrometry under multiple reaction monitoring mode,and quantified by standard solution.The results showed the method had good linearity( R≥0. 997) from 0. 01 ～ 1. 00 mg·L~(-1).Average fortified recoveries in samples were found in the range of 70. 6% ～ 105. 8%at three fortified levels from 0. 05 to 1. 00 mg·kg~(-1),with relative standard deviations of 0. 3% ～7. 9%( n= 5). The limits of detection( LOD) of cyhalofop-butyl and cyhalofop-caid were 0. 11 and 0. 16 μg·kg~(-1),while limits of quantification( LOQ) were 0. 37 and 0. 54μg·kg~(-1).The method is rapid and simple with high sensitivity and good reproducibility,and suitable for determination of cyhalofop-butyl and cyhalofop-caid in different matrix.
A method was developed for the simultaneous determination of cyhalofop-butyl and cyhalofop-caid in rice plant,rice,rice hull,paddyfield water and paddyfield soil.The residues were extracted from samples with acetonitrile and cleaned up with dispersive method on PSA,GCB and C18,then detected by ultra liquidchromatography-mass spectrometry under multiple reaction monitoring mode,and quantified by standard solution.The results showed the method had good linearity( R≥0. 997) from 0. 01 ～ 1. 00 mg·L~(-1).Average fortified recoveries in samples were found in the range of 70. 6% ～ 105. 8%at three fortified levels from 0. 05 to 1. 00 mg·kg~(-1),with relative standard deviations of 0. 3% ～7. 9%( n= 5). The limits of detection( LOD) of cyhalofop-butyl and cyhalofop-caid were 0. 11 and 0. 16 μg·kg~(-1),while limits of quantification( LOQ) were 0. 37 and 0. 54μg·kg~(-1).The method is rapid and simple with high sensitivity and good reproducibility,and suitable for determination of cyhalofop-butyl and cyhalofop-caid in different matrix.
引文
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[6]魏凤,杨仁斌,蒋波,等.高效液相色谱法测定稻田中的氰氟草酯[J].环境监测管理与技术,2015,27(5):45-48.
[7]赵莉,朱国念,姜忠涛,等.氰氟草酯及其代谢物在稻田水、土壤和稻株中的残留分析方法[J].分析化学,2003,31(2):163-166.
[8]董婷,罗泽江.超高效液相色谱法测定稻田水和土壤中氰氟草酯及其代谢产物[J].广州化工,2017,45(10):100-102.
[9]戴色琴,夏雪艳,黄挺,等.五氟磺草胺·氰氟草酯11.5%悬浮剂高效液相色谱分析方法的研究[J].中国农业信息,2014,(7):133-133.
[10]邵辉,张玉婷,李娜,等.GC/MS法测定大米中的精噁唑禾草灵和氰氟草酯残留量[J].分析实验室,2012,31(3):97-100.
[11]孙明娜,王梅,余璐,等.基质分散固相?液质联用法检测稻田水和土壤中氰氟草酯和双草醚残留[J].环境化学,2017,36(3):691-694.
[12]甘静妮,程雪梅,莫晓君分.散固相萃取/气相色谱-三重四极杆串联质谱测定蔬菜和水果中67种农药残留[J].分析测试学报,2016,35(12):1528-1534.
[2]Pinna M V,Braschi I,Blasioli S,et al.Hydrolysis and adsorptionof cyhalofop-butyl and cyhalofop-acid on soil colloids[J].J Agric Food Chem,2008,56:5273-5277.
[3]赵莉,樊晓青,朱国念,等.氰氟草酯水解动力学研究[J].农药学学报,2009,11(2):274-278.
[4]黄帆,郭正元,徐珍,等.氰氟草酯·精噁唑禾草灵混剂在水体中的残留分析方法[J].农药,2007,46(4):248-249.
[5]郭正元,黄帆,徐珍,等.10%精噁唑禾草灵·氰氟草酯乳油在水稻上的残留动态[J].生态农村环境学报,2008,24(1):51-54.
[6]魏凤,杨仁斌,蒋波,等.高效液相色谱法测定稻田中的氰氟草酯[J].环境监测管理与技术,2015,27(5):45-48.
[7]赵莉,朱国念,姜忠涛,等.氰氟草酯及其代谢物在稻田水、土壤和稻株中的残留分析方法[J].分析化学,2003,31(2):163-166.
[8]董婷,罗泽江.超高效液相色谱法测定稻田水和土壤中氰氟草酯及其代谢产物[J].广州化工,2017,45(10):100-102.
[9]戴色琴,夏雪艳,黄挺,等.五氟磺草胺·氰氟草酯11.5%悬浮剂高效液相色谱分析方法的研究[J].中国农业信息,2014,(7):133-133.
[10]邵辉,张玉婷,李娜,等.GC/MS法测定大米中的精噁唑禾草灵和氰氟草酯残留量[J].分析实验室,2012,31(3):97-100.
[11]孙明娜,王梅,余璐,等.基质分散固相?液质联用法检测稻田水和土壤中氰氟草酯和双草醚残留[J].环境化学,2017,36(3):691-694.
[12]甘静妮,程雪梅,莫晓君分.散固相萃取/气相色谱-三重四极杆串联质谱测定蔬菜和水果中67种农药残留[J].分析测试学报,2016,35(12):1528-1534.