食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
4期
1122-1127
,共6页
史晓梅%陈士恒%章晴%高丁%杨永坛
史曉梅%陳士恆%章晴%高丁%楊永罈
사효매%진사항%장청%고정%양영단
有机氯农药%拟除虫菊酯农药%固相萃取%气相色谱法%玉米
有機氯農藥%擬除蟲菊酯農藥%固相萃取%氣相色譜法%玉米
유궤록농약%의제충국지농약%고상췌취%기상색보법%옥미
organic chlorine pesticides%pyrethroid pesticides%solid phase extraction%gas chromatography%corn
目的:建立气相色谱-电子捕获检测器法(GC-ECD)测定玉米中16种有机氯和拟除虫菊酯农药残留量的方法。方法玉米样品经乙腈超声提取后,使用Florisil进行固相萃取净化,样品经氮吹浓缩后,使用气相色谱电子捕获检测器测定。结果16种有机氯和拟除虫菊酯农药在0.01~0.5 mg/L浓度范围内呈现良好线性关系, R2大于0.99;在0.02、0.05、0.2 mg/kg三个添加浓度上回收率范围为71.0%~103%,相对标准偏差1.28%~8.74%,检出限在0.1~16μg/kg之间。结论该方法前处理操作快速简单,能够有效净化样品,满足玉米中有机氯和拟除虫菊酯农药的日常检测和监管工作,适用于大批次样品的定性定量分析。
目的:建立氣相色譜-電子捕穫檢測器法(GC-ECD)測定玉米中16種有機氯和擬除蟲菊酯農藥殘留量的方法。方法玉米樣品經乙腈超聲提取後,使用Florisil進行固相萃取淨化,樣品經氮吹濃縮後,使用氣相色譜電子捕穫檢測器測定。結果16種有機氯和擬除蟲菊酯農藥在0.01~0.5 mg/L濃度範圍內呈現良好線性關繫, R2大于0.99;在0.02、0.05、0.2 mg/kg三箇添加濃度上迴收率範圍為71.0%~103%,相對標準偏差1.28%~8.74%,檢齣限在0.1~16μg/kg之間。結論該方法前處理操作快速簡單,能夠有效淨化樣品,滿足玉米中有機氯和擬除蟲菊酯農藥的日常檢測和鑑管工作,適用于大批次樣品的定性定量分析。
목적:건립기상색보-전자포획검측기법(GC-ECD)측정옥미중16충유궤록화의제충국지농약잔류량적방법。방법옥미양품경을정초성제취후,사용Florisil진행고상췌취정화,양품경담취농축후,사용기상색보전자포획검측기측정。결과16충유궤록화의제충국지농약재0.01~0.5 mg/L농도범위내정현량호선성관계, R2대우0.99;재0.02、0.05、0.2 mg/kg삼개첨가농도상회수솔범위위71.0%~103%,상대표준편차1.28%~8.74%,검출한재0.1~16μg/kg지간。결론해방법전처리조작쾌속간단,능구유효정화양품,만족옥미중유궤록화의제충국지농약적일상검측화감관공작,괄용우대비차양품적정성정량분석。
Objective To develop a method for the simultaneous determination of organic chlorine and pyrethroid pesticides residues in corn by gas chromatography with ECD detector.Methods Corn samples were extracted with acetonitrile by ultra-sonic, and the extracts were purified by solid phase extraction using Florisil, then samples were detected by GC-ECD after concentrated by nitrogen flushing.ResultsThe method showed a good linearity in the range of 0.01~0.5 mg/L for organic chlorine and pyrethroid pesticides with R2>0.99. The recoveries were in the range of 71.0%~103% at 3 spiked levels of 0.02, 0.05, and 0.2 mg/kg for organic chlorine and pyrethroid pesticides, and the relative standard deviations (RSDs) were 1.28%~8.74%. The limit of detection was in the range of 0.1~16μg/kg.Conclusion The method is suitable for quantitative and qualitative determination of organic chlorine and pyrethroid pesticides residues in a large number of corn samples with a sample and fast pretreatment procedure. Meanwhile, samples can be effectively cleaned up, and it could meet the requirements of daily inspection and supervision work.