分散固相萃取-超高效液相色谱串联质谱法测定土壤中噻唑磷残留
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摘要
[目的]建立土壤中噻唑磷的超高效液相色谱串联质谱法(UPLC-MS/MS)进行残留测定。[方法]土壤样品采用乙腈提取和PSA+C_(18)分散固相萃取,采用UPLC-MS/MS多反应模式(MRM)进行分析测定。[结果]噻唑磷添加水平在0.1~10μg范围内,平均回收率为94.3%~107.5%,相对标准偏差为7.9%~11.0%。采用外标法定量,方法的检出限为0.001 mg/L,定量限为0.005 mg/kg。[结论]该方法简单、准确、重复性较好且节省溶剂,适用于土壤环境中噻唑磷的残留检测。
[Aims] The aims were to establish a method for the determination of fosthiazate residues in soil by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). [Methods] The soil samples were extracted with acetonitrile, purified by PSA+C_(18)and analyzed by UPLC-MS/MS under the multiple reaction monitoring(MRM) mode. [Results] When the fortified level was 0.1-10 μg, the average recovery ranged from 94.3 to 107.5%with the relative standard deviation(RSD) was 7.9-11.0%. The quantitative analysis was performed by using external standard method.The limit of detection was 0.001 mg/L, and the limit of quantification was 0.005 mg/kg.[Conclusions] This method has the advantage of simple, accurate, good repeatability and solvent saving, which is suitable for the determination of fosthiazate residues in soil.
[Aims] The aims were to establish a method for the determination of fosthiazate residues in soil by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). [Methods] The soil samples were extracted with acetonitrile, purified by PSA+C_(18)and analyzed by UPLC-MS/MS under the multiple reaction monitoring(MRM) mode. [Results] When the fortified level was 0.1-10 μg, the average recovery ranged from 94.3 to 107.5%with the relative standard deviation(RSD) was 7.9-11.0%. The quantitative analysis was performed by using external standard method.The limit of detection was 0.001 mg/L, and the limit of quantification was 0.005 mg/kg.[Conclusions] This method has the advantage of simple, accurate, good repeatability and solvent saving, which is suitable for the determination of fosthiazate residues in soil.
引文
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[9]PANG Nan-nan,WANG Tie-long,HU Ji-ye.Method Validation and Dissipation Kinetics of Four Herbicides in Maize and Soil Using Qu ECh ERS Sample Preparation and Liquid Chromatography Tandem Mass Spectrometry[J].Food Chemistry,2016,190(1):793-800.
[2]陈品三.杀线虫剂主要类型、特性及其作用机制[J].农药科学与管理,2001,22(2):33-35.
[3]秦曙,乔雄梧,王霞,等.气相色谱法检测22种基质中的4种二硫代氨基甲酸盐类农药残留[J].色谱,2010,28(12):1162-1167.
[4]马帅,冯晓元,韩平,等.分散固相萃取-超高效液相色谱串联质谱法测定土壤中雌酮、雌二醇和乙炔基雌二醇[J].食品安全质量检测学报,2016,7(2):505-510.
[5]张玉婷,郭永泽,刘磊,等.噻唑膦在西瓜及土壤中的残留动态研究[J].天津农业科学,2011,17(4):68-70.
[6]郭利丰,吴玉琴.噻唑膦的高效液相色谱分析[J].农药科学与管理,2013,34(2):40-42.
[7]ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,et al.Fast and Easy Multiresidue Method Employing Acetonitrile Extraction/Portioning and“Dispersive Solid-phase Extraction”for the Determination of Pesticide Residues in Produce[J].Journal of AOAC International,2003,86(2):412-431.
[8]ABDEL-GHANY M F,HUSSEIN L A,NFE AZAB,et al.Simultaneous Determination of Eight Neonicotinoid Insecticide Residues and Two Primary Metabolites in Cucumbers and Soil by Liquid Chromatography-tandem Mass Spectrometry Coupled with Qu ECh ER S[J].Journal of Chromatography B,2016,1031(15):15-28.
[9]PANG Nan-nan,WANG Tie-long,HU Ji-ye.Method Validation and Dissipation Kinetics of Four Herbicides in Maize and Soil Using Qu ECh ERS Sample Preparation and Liquid Chromatography Tandem Mass Spectrometry[J].Food Chemistry,2016,190(1):793-800.