粮油食品科技
糧油食品科技
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SCIENCE AND TECHNOLOGY OF CEREALS,OILS AND FOODS
2015年
4期
75-79
,共5页
徐明雅%潘丹杰%杨志成%张烝彦
徐明雅%潘丹傑%楊誌成%張烝彥
서명아%반단걸%양지성%장증언
分散固相萃取%气相色谱%稻谷%有机磷农药残留
分散固相萃取%氣相色譜%稻穀%有機燐農藥殘留
분산고상췌취%기상색보%도곡%유궤린농약잔류
dispersive solid phase extraction%gas chromatography(GC)%paddy%organophosphorus pes-ticide residues
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0.002 mg/kg,最低定量限(LOQ)为0.007 mg/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。
建立中性氧化鋁分散固相萃取—火燄光度氣相色譜法測定稻穀中樂果、毒死蜱、馬拉硫燐、水胺硫燐、三唑燐5種有機燐農藥殘留量的分析方法。樣品粉碎後經乙腈提取,中性氧化鋁分散萃取,萃取液于70℃水浴中氮吹榦,丙酮定容後用帶火燄光度檢測器的毛細管氣相色譜儀(GC -FPD)測定。結果錶明,5種有機燐在0.05~5.00μg/mL 範圍具有良好的線性關繫,樂果、毒死蜱、馬拉硫燐、水胺硫燐、三唑燐的線性相關繫數均為0.9999,檢齣限(LOD)為0.002 mg/kg,最低定量限(LOQ)為0.007 mg/kg。稻穀樣品中低、中、高3箇質量濃度的添加迴收率在97.7%~108.0%之間,相對標準偏差(RSD,n =6)在0.8%~5.7%之間。方法可以滿足稻穀中5種有機燐農藥殘留一次處理同時分析檢測的要求。
건립중성양화려분산고상췌취—화염광도기상색보법측정도곡중악과、독사비、마랍류린、수알류린、삼서린5충유궤린농약잔류량적분석방법。양품분쇄후경을정제취,중성양화려분산췌취,췌취액우70℃수욕중담취간,병동정용후용대화염광도검측기적모세관기상색보의(GC -FPD)측정。결과표명,5충유궤린재0.05~5.00μg/mL 범위구유량호적선성관계,악과、독사비、마랍류린、수알류린、삼서린적선성상관계수균위0.9999,검출한(LOD)위0.002 mg/kg,최저정량한(LOQ)위0.007 mg/kg。도곡양품중저、중、고3개질량농도적첨가회수솔재97.7%~108.0%지간,상대표준편차(RSD,n =6)재0.8%~5.7%지간。방법가이만족도곡중5충유궤린농약잔류일차처리동시분석검측적요구。
A fast method was developed for the determination of 5 organophosphorus pesticide residues (dimethoate,chlorpyrifos,malathion,isocarbophos,fenitrothion)in paddy by neutral alumina disper-sive 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 mini-mum 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 meth-od could be used to determine 5 organophosphorus pesticide residues in paddy at the same time.