改良QuEChERS法测定土壤中的毒杀芬残留量
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摘要
[目的]建立毒杀芬在农田土壤中残留量的气相色谱检测方法。[方法]样品采用正己烷提取后,经PSA和Carb净化,气相色谱电子捕获检测器测定,外标法定量。[结果]方法定量限(S/N=10∶1)为0.01 mg/kg,在0.10～3.0 mg/L的质量浓度范围内,相关系数为0.998,在土壤中添加0.01～0.1 mg/kg范围内(n=6),回收率为75%～92%,相对标准偏差(RSD)为4.1%～5.4%。[结论]该方法适用于土壤中毒杀芬的快速检测。
[Aims] A method was developed for the determination of toxaphene residues in soil by capillary gas chromatographic. [Methods] The pesticide was extracted using n-hexane and purified by PSA and Carb, finally detected by GC-electron capture detector, external standard method for quantitative. [Results] The limit of quantitation(S/N=10∶1) was 0.01 mg/kg. In the linear range of 0.10-3.0 mg/L, the correlation coefficient was 0.998. In a range of 0.01-0.1 mg/kg(n=6), the corresponding recoveries were 75-92%, the relative standard deviations(RSD) were 4.1-5.4%.[Conclusions] The method is suitable for rapid detection of toxaphene residues in soil.
[Aims] A method was developed for the determination of toxaphene residues in soil by capillary gas chromatographic. [Methods] The pesticide was extracted using n-hexane and purified by PSA and Carb, finally detected by GC-electron capture detector, external standard method for quantitative. [Results] The limit of quantitation(S/N=10∶1) was 0.01 mg/kg. In the linear range of 0.10-3.0 mg/L, the correlation coefficient was 0.998. In a range of 0.01-0.1 mg/kg(n=6), the corresponding recoveries were 75-92%, the relative standard deviations(RSD) were 4.1-5.4%.[Conclusions] The method is suitable for rapid detection of toxaphene residues in soil.
引文
[1]VETTER W,OEHME M.Toxaphene Analysis and the Environmental Fate of Congeners[C]//New Types of Persistent Halogenated Compounds.Passivity J,ed.Berlin:Springer Press,2003(3):237-287.
[2]BIDLEMANA T F,CUSSIONB S,JANTUNENA L M.Interlaboratory Study of Toxaphene Analysis in Ambient Air[J].Atmospheric Environment,2004,38:3713-3722.
[3]LACAYORA M,BAVEL B,MATTIASSON B.Degradation of Toxaphene in Water During Anaerobic and Aerobic Conditions[J].Environmental Pollution,2004,130:437-443.
[4]谢原利,饶竹,王沫,等.毒杀芬的环境行为及检测研究进展[J].岩矿测试,2008,27(10):360-370.
[5]GB 2763—2016.食品安全国家标准食品中农药最大残留限量[S].
[6]田绍琼,毛秀红,苗水,等.气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量[J].色谱,2012,3(1):14-20.
[7]戴晖.微波萃取-毛细管气相色谱法快速分析土壤中有机氯农药[J].分析仪器,2004(2):3l-34.
[8]戴博,金红宇,张华峰,等.凝胶渗透色谱-固相萃取净化气相色谱-质谱法检测甘草、黄芪、人参和银杏叶中24种农药残留[J].药物分析杂志,2011,31(3):558-563.
[9]程寿峰.30种黔中药材饮片中11种有机氯农药残留的污染调查与研究[J].时珍国医国药,2013,24(9):2282-2290.
[10]SCHENCK F J,HOBBS J E.Evaluation of the Quick,Easy,Cheap,Effective,Rugged,and Safe(Qu ECh ERS)Approach Pesticide Residue Analysis[J].Bull Environ Contam Toxicol,2004,73(1):24-30.
[11]王明泰,刘志研,李爱军.纺织品的毒杀芬残留量测定[J].印染,2006,60:55-59.
[12]张慧丽,王建华,姜瑛,等.固相萃取-气相色谱-负化学源质谱法检测水果和蔬菜中的毒杀芬[J].化学分析计量,2016,25(5):53-67.
[2]BIDLEMANA T F,CUSSIONB S,JANTUNENA L M.Interlaboratory Study of Toxaphene Analysis in Ambient Air[J].Atmospheric Environment,2004,38:3713-3722.
[3]LACAYORA M,BAVEL B,MATTIASSON B.Degradation of Toxaphene in Water During Anaerobic and Aerobic Conditions[J].Environmental Pollution,2004,130:437-443.
[4]谢原利,饶竹,王沫,等.毒杀芬的环境行为及检测研究进展[J].岩矿测试,2008,27(10):360-370.
[5]GB 2763—2016.食品安全国家标准食品中农药最大残留限量[S].
[6]田绍琼,毛秀红,苗水,等.气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量[J].色谱,2012,3(1):14-20.
[7]戴晖.微波萃取-毛细管气相色谱法快速分析土壤中有机氯农药[J].分析仪器,2004(2):3l-34.
[8]戴博,金红宇,张华峰,等.凝胶渗透色谱-固相萃取净化气相色谱-质谱法检测甘草、黄芪、人参和银杏叶中24种农药残留[J].药物分析杂志,2011,31(3):558-563.
[9]程寿峰.30种黔中药材饮片中11种有机氯农药残留的污染调查与研究[J].时珍国医国药,2013,24(9):2282-2290.
[10]SCHENCK F J,HOBBS J E.Evaluation of the Quick,Easy,Cheap,Effective,Rugged,and Safe(Qu ECh ERS)Approach Pesticide Residue Analysis[J].Bull Environ Contam Toxicol,2004,73(1):24-30.
[11]王明泰,刘志研,李爱军.纺织品的毒杀芬残留量测定[J].印染,2006,60:55-59.
[12]张慧丽,王建华,姜瑛,等.固相萃取-气相色谱-负化学源质谱法检测水果和蔬菜中的毒杀芬[J].化学分析计量,2016,25(5):53-67.