摘要
建立中性氧化铝分散固相萃取-火焰光度气相色谱法测定稻谷中乐果、毒死蜱、马拉硫磷、水胺硫磷、三唑磷5种有机磷农药残留量的分析方法。样品粉碎后经乙腈提取,中性氧化铝分散萃取,萃取液于70℃水浴中氮吹干,丙酮定容后用带火焰光度检测器的毛细管气相色谱仪(GC—FPD)测定。结果表明,5种有机磷在0.05~5.00μg/mL范围具有良好的线性关系,乐果、毒死蜱、马拉硫磷、水胺硫磷、三唑磷的线性相关系数均为0.9999,检出限(LOD)为0.002mg/kg,最低定量限(LOQ)为0.007mg/kg。稻谷样品中低、中、高3个质量浓度的添加回收率在97.7%-108.0%之间,相对标准偏差(RSD,n=6)在0.8%-5.7%之间。方法可以满足稻谷中5种有机磷农药残留一次处理同时分析检测的要求。
A fast method was developed for the determination of 5 organophosphorus pesticide residues ( dimethoate, chlorpyrifos, malathion, isoearbophos, fenitrothion) in paddy by neutral alumina dispersive solid phase extraction - gas chromatography with flame photometric detector (DSPE -GC -FPD). The powdered samples were extracted with acetonitrile. The extract was purified by neutral alumina DSPE, dried by nitrogen evaporator with water bath at 70℃, and dissolved by acetone and determined by capillary gas chromatograph with flame photometric detector( CGC -FPD). The results showed that the 5 organophosphorus pesticide showed a good linear relationship in the range of 0.05 - 5.00 μg/mL, all of their linear correlation coefficients were 0.999 9, the limit of detection was 0.002 mg/kg, and the minimum quantitative limit was 0. 007 mg,/kg. The spiked recoveries at three levels of standard additions in paddy were between 97.7%- 108.0% , and the RSDs ( n = 6) were between 0.8% - 5.7%. This method could be used to determine 5 organophosphorus pesticide residues in paddy at the same time.
出处
《粮油食品科技》
2015年第4期75-79,共5页
Science and Technology of Cereals,Oils and Foods
关键词
分散固相萃取
气相色谱
稻谷
有机磷农药残留
dispersive solid phase extraction
gas chromatography(GC)
paddy
organophosphorus pesticide residues