摘要
建立同时测定稻田土壤中的EPTC(茵草敌)、禾草敌、毒草胺、丁氟消草、氟草胺、灭草灵除草剂残留的全自动固相萃取(SPE)联合气相色谱-三重四级杆串联质谱(GC-MS/MS)的分析方法。采用全自动固相萃取技术,选择乙酸乙酯+二氯甲烷(1+1)作为提取溶剂,以ENVI–Carb固相萃取柱对稻田土壤中的除草剂残留进行富集,处理后的样品进样气相色谱质谱系统,选择多反应监测模式(MRM)扫描,外标法定量。6种杀虫剂的线性范围为0.05~5.0μg/mL,线性相关系数均大于0.995,检出限均在0.006~0.016μg/kg之间。在0.1mg/kg,0.5 mg/kg和2.0 mg/kg 3水平加标测试下,6种农药残留的加标回收率均在86.2%~108.6%之间,精密度测定结果的变异系数(相对标准偏差,RSD)范围1.89%~4.05%(n=6)。该方法前处理简单,灵敏度高,定性定量结果准确,适用于土壤中农药残留的监测。于土壤中农药残留的监测。
An ananytical method was developed for detection of 6 herbicides(EPTC,molinate,propachlor,ethalfluralin,acetochlor,benfluralin and swep)residues in paddy soil using automatic solid phase extraction(SPE)plus gas chromatography-tandem mass spectrometry(GC-MS/MS).Using automatic solid phase extraction technology,ethyl acetate+dichloromethane(1+1)was selected as the extraction solvent,Envi-Carb solid phase extraction column was used to enrich herbicide residues in paddy soil.After treatment,samples were injected into the gas chromatography-mass spectrometry system,multi-reaction monitoring mode(MRM)scanning was selected and quantified by external standard method.The linear range of 6 herbicides were 0.05-5.0μg/mL,with correlation coefficients were all above 0.995.Their detection limits were in the range 0.006-0.016μg/kg,Recoveries of the 6 pesticides at 3 spiked concentration level,0.1,0.5 and 2.0 mg/kg,varied from 86.2%to 108.6%,with relative standard deviations(RSD)of precision ranged from 1.89%to 4.05%.This method has the advantages of simple pretreatment,high sensitivity,accurate qualitative and quantitative results,and is suitable for the monitoring of pesticide residues in soil.
作者
郭伟伟
孙志洪
卢冠宇
张淑华
GUO Weiwei;SUN Zhihong;LU Guanyu;ZHANG Shuhua(Cangzhou Ecological Environment Monitoring Center,Cangzhou 061000,China;Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China;Guodian United Power Technology Co.,Ltd.,Beijing 100000,China;Hebei Qinghong Testing Technology Service Co.,Ltd.,Cangzhou 061000,China)
出处
《中国测试》
CAS
北大核心
2022年第11期78-81,119,共5页
China Measurement & Test
