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
1498-1503
,共6页
刘会双%冯刚%刘萍%刘晓慧%冉升
劉會雙%馮剛%劉萍%劉曉慧%冉升
류회쌍%풍강%류평%류효혜%염승
干辣椒%农药残留%气相色谱质谱法%检测
榦辣椒%農藥殘留%氣相色譜質譜法%檢測
간랄초%농약잔류%기상색보질보법%검측
dry chilli%pesticide residue%gas chromatography-mass spectrometry%determination
目的:建立凝胶色谱技术(GPC)净化和气相色谱质谱法同时测定干辣椒中常用有机磷和拟除虫菊酯类农药的测定方法。方法样品采用乙腈-水提取,经凝胶色谱仪净化去除大分子色素及杂质,再经过石墨化炭黑-氨基SPE柱净化,以气相色谱-质谱联用仪(EI源)检测,内标法定量。结果在添加水平为0.05~0.5 mg/kg下的平均回收率为71.6%~116.4%,相对标准偏差在2.3%~10.8%之间,样品最低检出限为0.01~0.05 mg/kg。结论此方法净化效果显著,测定结果准确,实验周期短,基本实现全自动化,节省大量时间与试剂,适用于大批量辣椒的农药残留检测。
目的:建立凝膠色譜技術(GPC)淨化和氣相色譜質譜法同時測定榦辣椒中常用有機燐和擬除蟲菊酯類農藥的測定方法。方法樣品採用乙腈-水提取,經凝膠色譜儀淨化去除大分子色素及雜質,再經過石墨化炭黑-氨基SPE柱淨化,以氣相色譜-質譜聯用儀(EI源)檢測,內標法定量。結果在添加水平為0.05~0.5 mg/kg下的平均迴收率為71.6%~116.4%,相對標準偏差在2.3%~10.8%之間,樣品最低檢齣限為0.01~0.05 mg/kg。結論此方法淨化效果顯著,測定結果準確,實驗週期短,基本實現全自動化,節省大量時間與試劑,適用于大批量辣椒的農藥殘留檢測。
목적:건립응효색보기술(GPC)정화화기상색보질보법동시측정간랄초중상용유궤린화의제충국지류농약적측정방법。방법양품채용을정-수제취,경응효색보의정화거제대분자색소급잡질,재경과석묵화탄흑-안기SPE주정화,이기상색보-질보련용의(EI원)검측,내표법정량。결과재첨가수평위0.05~0.5 mg/kg하적평균회수솔위71.6%~116.4%,상대표준편차재2.3%~10.8%지간,양품최저검출한위0.01~0.05 mg/kg。결론차방법정화효과현저,측정결과준학,실험주기단,기본실현전자동화,절성대량시간여시제,괄용우대비량랄초적농약잔류검측。
Objective A novel method was established to detect organophosphorus and pyrethroid pesticide residues in dry chillies by gel permeation chromatography (GPC) and gas chromatography mass spectrometry simultaneously.Methods The sample was extracted by acetonitrile-water, purified by GPC (dislodging macromolecular pigment as well as impurities) and an SPE graphitized carbon black-amino column, and simultaneously detected by gas chromatography-mass spectrometry (GC-MS) with internal standard method for quantification.Result The average recovery was 71.6%~116.4% at spiked level of 0.05~0.5 mg/kg and the relative standard deviation was 2.3%~10.8%. Limit of minimum detection was 0.01~0.05 mg/kg.Conclusion Compared with reported methods, this method had advantages of remarkable purification, accurate determination, short running time by full automation and fewer use of reagent. It was a powerful complement for the detection of pesticide residues for large quantities of pepper.