色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
10期
1131-1137
,共7页
黄倩%何蔓%陈贝贝%胡斌
黃倩%何蔓%陳貝貝%鬍斌
황천%하만%진패패%호빈
磁固相萃取%气相色谱-火焰光度检测%有机磷农药%果汁
磁固相萃取%氣相色譜-火燄光度檢測%有機燐農藥%果汁
자고상췌취%기상색보-화염광도검측%유궤린농약%과즙
magnetic solid phase extraction( MSPE)%gas chromatography-flame photometric detection( GC-FPD)%organophosphorus pesticides( OPPs)%juices
制备了苯乙烯(St)和甲基丙烯酸(MAA)共聚物改性的磁性微球 Fe3O4@P(St-co-MAA),并将其作为磁固相萃取吸附剂,建立了磁固相萃取(MSPE)-气相色谱(GC)-火焰光度检测(FPD)联用分析有机磷农药(OPPs)残留的新方法。以5种有机磷农药(二嗪农、甲基毒死蜱、杀螟硫磷、毒死蜱和喹硫磷)为目标分析物,考察并优化了吸附和解吸条件,确定了最佳实验条件。在最优的实验条件下,方法对5种 OPPs 的检出限( S/N=3)为0.013~0.305μg/L,方法的相对标准偏差( RSD,n=7)为3.1%~8.8%,富集倍数为406~951,线性范围达3个数量级。将该方法应用于新鲜番茄汁、草莓汁样品中的 OPPs 残留分析,加标回收率为85.4%~118.9%。该方法具有检出限低、分析速度快、富集倍数高等优点,为有机磷农药的残留分析提供了新的技术平台。
製備瞭苯乙烯(St)和甲基丙烯痠(MAA)共聚物改性的磁性微毬 Fe3O4@P(St-co-MAA),併將其作為磁固相萃取吸附劑,建立瞭磁固相萃取(MSPE)-氣相色譜(GC)-火燄光度檢測(FPD)聯用分析有機燐農藥(OPPs)殘留的新方法。以5種有機燐農藥(二嗪農、甲基毒死蜱、殺螟硫燐、毒死蜱和喹硫燐)為目標分析物,攷察併優化瞭吸附和解吸條件,確定瞭最佳實驗條件。在最優的實驗條件下,方法對5種 OPPs 的檢齣限( S/N=3)為0.013~0.305μg/L,方法的相對標準偏差( RSD,n=7)為3.1%~8.8%,富集倍數為406~951,線性範圍達3箇數量級。將該方法應用于新鮮番茄汁、草莓汁樣品中的 OPPs 殘留分析,加標迴收率為85.4%~118.9%。該方法具有檢齣限低、分析速度快、富集倍數高等優點,為有機燐農藥的殘留分析提供瞭新的技術平檯。
제비료분을희(St)화갑기병희산(MAA)공취물개성적자성미구 Fe3O4@P(St-co-MAA),병장기작위자고상췌취흡부제,건립료자고상췌취(MSPE)-기상색보(GC)-화염광도검측(FPD)련용분석유궤린농약(OPPs)잔류적신방법。이5충유궤린농약(이진농、갑기독사비、살명류린、독사비화규류린)위목표분석물,고찰병우화료흡부화해흡조건,학정료최가실험조건。재최우적실험조건하,방법대5충 OPPs 적검출한( S/N=3)위0.013~0.305μg/L,방법적상대표준편차( RSD,n=7)위3.1%~8.8%,부집배수위406~951,선성범위체3개수량급。장해방법응용우신선번가즙、초매즙양품중적 OPPs 잔류분석,가표회수솔위85.4%~118.9%。해방법구유검출한저、분석속도쾌、부집배수고등우점,위유궤린농약적잔류분석제공료신적기술평태。
A novel method for the determination of organophosphorous pesticides( OPPs)in fresh juice samples was developed. Fe3O4@ P( St-co-MAA)magnetic microparticles were syn-thesized and modified with styrene( St)and methacrylic acid( MAA)by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3O4 magnetic nanoparticles(MNPs)have been successfully modified with St and MAA. Based on the prepared Fe3O4@ P( St-co-MAA)magnetic microparticles,a novel method of magnetic solid phase extraction( MSPE)-gas chromatography( GC)-flame photometric detection( FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized,and the analytical performance was evaluated under the optimal conditions. The limits of detection( LODs,S/N=3)for target OPPs were in the range of 0. 013-0. 305 μg/L with the RSDs(n=7)ranging from 3. 1% to 8. 8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes( R2﹥0. 99)and the reproducibil-ities were 7. 4%-14. 5%( n=5). Finally,the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples,with the recoveries of target OPPs in the range of 85. 4%-118. 9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost,fast separation and high enrichment factor.