快速溶剂萃取-GC-MS/MS法测定经济作物土壤中的甲霜灵、嘧霉胺、戊唑醇等6种常用农药残留
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摘要
建立一种利用快速溶剂萃取(ASE)-气相色谱-三重四级杆质谱仪检测经济作物土壤中甲霜灵、嘧霉胺、戊唑醇等6种农药的分析方法。样品经研钵研细,利用ASE进行提取,提取液经氮吹浓缩后,上GC-MS/MS进行检测,外标法定量。6种农药质量浓度在0.05～5μg/mL范围内线性关系良好,相关系数均大于0.995;检出限在0.005～0.023μg/mL;加标回收率在81.2%～108.7%之间;重复性(n=6)相对标准偏差在3.26%～4.40%之间。实验表明该方法具有操作简单、检测速度快、检出限低等优点,适用于经济作物土壤中多种农药残留的分析检测。
A ASE(accelerated solvent extraction)-GC/MS/MS method for determination of 6 common pesticides residuals such as pyrimethani, metalaxyl, thiamethoxam, et al in economic crop soil was established.Soil samples were grinded in mortar, then extracted by ASE, The exracted solution were dryed under nitrogen,then samples were analyzed by GC-MS/MS. External standard was used as quantitative method. The concentration of 6 pesticides showed good linear relationships in the range 0.05-5 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.005 and 0.023 mg/kg, and the recoveries were ranged from 81.2% to 108.7%. The relative standard deviation(RSD)of Repeatability(n=6)were 3.26%-4.40%. This method was proved to be simple and quick treated, and with low detection, which can be used to determine pesticide residues in economic crop soil.
A ASE(accelerated solvent extraction)-GC/MS/MS method for determination of 6 common pesticides residuals such as pyrimethani, metalaxyl, thiamethoxam, et al in economic crop soil was established.Soil samples were grinded in mortar, then extracted by ASE, The exracted solution were dryed under nitrogen,then samples were analyzed by GC-MS/MS. External standard was used as quantitative method. The concentration of 6 pesticides showed good linear relationships in the range 0.05-5 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.005 and 0.023 mg/kg, and the recoveries were ranged from 81.2% to 108.7%. The relative standard deviation(RSD)of Repeatability(n=6)were 3.26%-4.40%. This method was proved to be simple and quick treated, and with low detection, which can be used to determine pesticide residues in economic crop soil.
引文
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[8]魏进,张盈,李汶锟.QuEChERS-超高效液相色谱-电喷雾串联质谱法测定小麦籽粒、植株和土壤中氯啶菌酯残留[J].山东农业科学,2016,48(4):124-128.
[9]吴小春,姚科伟,魏双利,等.快速溶剂萃取-气相色谱质谱法测定土壤中戊唑醇残留量[J].化学分析计量,2015,24(3):76-78.
[10]江泽军,张鹏,李永飞,等.分散固相萃取-高效液相色谱-串联质谱法测定水稻和土壤中的福美双与甲霜灵残留[J].农药学学报,2015,17(3):313-320.
[2]王建伟,张彩香,潘真真,等.江汉平原典型土壤环境中有机磷农药的分布特征及影响因素[J].中国环境科学,2016,36(10):3089-3098.
[3]陈芳,杨艳,高辉,等.腐殖质吸附有机农药机理研究进展[J].四川环境,2017,36(6):141-149.
[4]吴琼,罗金辉,谢德芳,等.戊唑醇在香蕉中的残留动态研究及风险评估[J].陕西农业科学,2015, 61(11):22-25.
[5]吕晓峰,李艳,陈梦静,等.农药残留对农产品质量安全的影响与应对措施[J].安徽农业科学,2016,44(33):131-134.
[6]刘磊,李辉,邵辉,等.超高效液相色谱-串联质谱法测定辣椒及其栽培土壤中烯酰吗啉和唑嘧菌胺[J].食品安全质量检测学报,2017(8):2983-2988.
[7]张爱娟,梁林,翟淑华,等.超高效液相色谱串联质谱法检测辣椒及土壤中啶氧菌酯的残留[J].农药科学与管理,2016(10):40-43.
[8]魏进,张盈,李汶锟.QuEChERS-超高效液相色谱-电喷雾串联质谱法测定小麦籽粒、植株和土壤中氯啶菌酯残留[J].山东农业科学,2016,48(4):124-128.
[9]吴小春,姚科伟,魏双利,等.快速溶剂萃取-气相色谱质谱法测定土壤中戊唑醇残留量[J].化学分析计量,2015,24(3):76-78.
[10]江泽军,张鹏,李永飞,等.分散固相萃取-高效液相色谱-串联质谱法测定水稻和土壤中的福美双与甲霜灵残留[J].农药学学报,2015,17(3):313-320.