摘要
建立全自动固相萃取(SPE)净化大棚种植土壤中的嘧菌酯、肟菌酯、霜霉威、甲霜灵和烯酰吗啉杀菌剂的GC-MS/MS快速检测方法。土壤样品自然晾干,碾碎,经乙腈萃取后,于全自动固相萃取仪上净化,收集净化液并经氮气吹至近干。残渣用正己烷定容至1 mL,于气相色谱三重四级杆串联质谱仪分析,外标法定量。在0.04~4.0μg/mL实验浓度范围内,5种杀菌剂质量浓度与对应的峰面积呈良好的线性关系,相关系数均大于0.995,检出限均在0.0014~0.0042 mg/kg范围内。3个不同浓度水平平均加标回收率在89.8%~103.2%之间,精密度测试结果的相对标准偏差均小于5%(n=6)。方法实用性强,定性定量结果准确、可靠,适用于土壤样品中农药残留的监测。
To establish a GC-MS/MS method for rapid determination of azoxystrobin,oximectin,flumetoclopramide,metalaxyl and enylmorpholine in greenhouse soil by solid-phase extraction.The soil samples were dried and crushed.After extraction by acetonitrile,it was purified on the full-automatic solid-phase extractor,and the purified liquid is collected and blown to near dry by nitrogen.The residue was fixed with 1 mL n-hexane,which analyzed by gas chromatography triple quadrupole tandem mass spectrometer and quantified by external standard method.The mass concentration of five fungicides had a good linear relationship in range of 0.04~4.0μg/mL with the corresponding peak area.The correlation coefficient was greater than 0.995.The detection limit was in range of 0.0014~0.0042 mg/kg.The average recovery of three different concentration levels was between 89.8%and 103.2%.The relative standard deviation of the precision test results was less than 5%(n=6).The method was practical,accurate and reliable,and was suitable for the monitoring of pesticide residues in soil samples.
作者
吴伟
杨彬
张翠华
WU Wei;YANG Bin;ZHANG Cui-hua(Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China;School of Chemistry and Chemical Engineering,Cangzhou Normal University,Cangzhou 061001,China)
出处
《化学试剂》
CAS
北大核心
2020年第10期1186-1189,共4页
Chemical Reagents
