烟草科技
煙草科技
연초과기
TOBACCO SCIENCE & TECHNOLOGY
2015年
5期
47-56
,共10页
余斐%陈黎%艾丹%潘立宁%胡斌%刘惠民
餘斐%陳黎%艾丹%潘立寧%鬍斌%劉惠民
여비%진려%애단%반립저%호빈%류혜민
多壁碳纳米管%烟草%农药残留%液相色谱-串联质谱%QuEChERS
多壁碳納米管%煙草%農藥殘留%液相色譜-串聯質譜%QuEChERS
다벽탄납미관%연초%농약잔류%액상색보-천련질보%QuEChERS
Multi-walled carbon nanotube%Tobacco%Pesticide residue%LC-MS/MS%QuEChERS
建立了一种以多壁碳纳米管(MWCNTs)为吸附剂的分散固相萃取(DSPE)、液相色谱-串联质谱(LC-MS/MS)测定烟草中114种农药残留的分析方法。通过优化实验,选择并确定了MWCNTs的型号和用量,在QuEChERS方法的基础上改善了样品净化效果。结果表明:①以外径>50 nm、用量5 mg的MWCNTs为净化剂材料,可以获得比N-丙基乙二胺(PSA)更好的净化效果。②工作曲线线性良好(r2>0.999),3个添加水平(0.02,0.05,0.20 mg/kg)的平均回收率为69%~119%,相对标准偏差为1%~19%,方法定量限(LOQ)在0.2~40.0μg/kg之间。该方法准确度高、灵敏度好、操作简便,适合用于烟草样品中114种农药残留的检测。
建立瞭一種以多壁碳納米管(MWCNTs)為吸附劑的分散固相萃取(DSPE)、液相色譜-串聯質譜(LC-MS/MS)測定煙草中114種農藥殘留的分析方法。通過優化實驗,選擇併確定瞭MWCNTs的型號和用量,在QuEChERS方法的基礎上改善瞭樣品淨化效果。結果錶明:①以外徑>50 nm、用量5 mg的MWCNTs為淨化劑材料,可以穫得比N-丙基乙二胺(PSA)更好的淨化效果。②工作麯線線性良好(r2>0.999),3箇添加水平(0.02,0.05,0.20 mg/kg)的平均迴收率為69%~119%,相對標準偏差為1%~19%,方法定量限(LOQ)在0.2~40.0μg/kg之間。該方法準確度高、靈敏度好、操作簡便,適閤用于煙草樣品中114種農藥殘留的檢測。
건립료일충이다벽탄납미관(MWCNTs)위흡부제적분산고상췌취(DSPE)、액상색보-천련질보(LC-MS/MS)측정연초중114충농약잔류적분석방법。통과우화실험,선택병학정료MWCNTs적형호화용량,재QuEChERS방법적기출상개선료양품정화효과。결과표명:①이외경>50 nm、용량5 mg적MWCNTs위정화제재료,가이획득비N-병기을이알(PSA)경호적정화효과。②공작곡선선성량호(r2>0.999),3개첨가수평(0.02,0.05,0.20 mg/kg)적평균회수솔위69%~119%,상대표준편차위1%~19%,방법정량한(LOQ)재0.2~40.0μg/kg지간。해방법준학도고、령민도호、조작간편,괄합용우연초양품중114충농약잔류적검측。
A method combining dispersive solid phase extraction (DSPE), wherein multi-walled carbon nanotubes (MWCNTs) were used as adsorption material, with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for simultaneously determining 114 pesticide residues in tobacco. The type and adding rate of MWCNTs were optimized by experiments, and the purification of samples was improved by QuEChERS method. The results showed that: 1) It was more efficient using 5 mg MWCNTs of above 50 nm in external diameter than using N-Propylethane-1,2-diamine (PSA) in sample purification. 2) The calibration curve presented good linearity (r2>0.999). The average recoveries at spiked levels of 0.02, 0.05 and 0.20 mg/kg ranged from 69% to 119% with the relative standard deviations of 1%-19%, and the LOQs of the method were in the range of 0.2-40.0 g/kg. The developed method is accurate, sensitive, convenient, and suitable.