摘要
采用溶剂热反应法一步合成制备出石墨烯基铁氧化物磁性材料（G-Fe3O4），将其作为磁固相萃取吸附剂，通过优化样品提取液稀释比例、萃取材料用量、萃取时间、洗脱剂的种类和体积等条件，并结合气相色谱-串联质谱（GC-MS/MS）技术，建立了花生样品中9种常用农药多残留的检测方法。结果表明，该方法对9种农药的检出限为0.07~1.85μg/kg，线性范围为0.23~1000μg/kg，相关系数（r2）均不低于0.994；在低、中、高3个不同加标水平下的平均回收率为81.9%~119.3%，相对标准偏差（RSD）为2.1%~6.6%。该方法简便易行、回收率高、稳定性好、成本低，为花生等高油脂复杂基质中农药多残留检测提供了一种快捷、高效、准确的分析方法。
G-Fe3O4 magnetic composite materials with excellent adsorption properties were successfully synthesized by solvothermal method,and then applied in magnetic solid phase extraction（MSPE） process for 9 common pesticides in peanut samples.The extraction conditions were optimized,such as dilution ratio of sample extract,amount of magnetic composite materials,extraction time,type and dosage of elution solvent.Coupled with gas chromatography-tandem mass spectrometry（GC-MS/MS）,a novel multi-residue analytical method was established for these nine pesticides in complex peanut matrix.The results showed that the limits of detection for nine pesticides ranged from 0.07μg/kg to 1.85μg/kg,the linear ranges were 0.23-1000μg/kg,and the correlation coefficients（r2） were not less than 0.994.The average recoveries at three spiked levels ranged from 81.9% to 119.3%,with relative standard deviations（RSD） of 2.1%-6.6%.With the advantages of simple operation,high recovery,good stability and low cost,this method was a rapid,efficient and accurate technique for multi-residue determination of pesticide,especially in high fatty matrix such as peanut sample.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第9期1087-1093,共7页
Journal of Instrumental Analysis
基金
国家自然科学基金(31471650)
公益性农业行业科研专项课题(201203037-05,201203094)
国家农产品质量安全风险评估重大项目(GJFP2016007)
关键词
磁固相萃取
气相色谱-串联质谱
农药残留
花生
magnetic solid phase extraction（MSPE）
gas chromatography tandem mass spectrometry（GC-MS/MS）
pesticide residues
peanut
