安徽农学通报
安徽農學通報
안휘농학통보
AUHUI AGRICULTURAL SCIENCE BULLETIN
2014年
22期
129-134
,共6页
蒋治国%王博超%殷雪琰%堵燕钰%罗漪涟
蔣治國%王博超%慇雪琰%堵燕鈺%囉漪漣
장치국%왕박초%은설염%도연옥%라의련
在线凝胶渗透色谱/气相色谱-串联质谱%QuEChERS法%农药残留%蔬菜
在線凝膠滲透色譜/氣相色譜-串聯質譜%QuEChERS法%農藥殘留%蔬菜
재선응효삼투색보/기상색보-천련질보%QuEChERS법%농약잔류%소채
Online gel permeation chromatography/gas chromatography-tandem mass spectrometry%QuECh-ERS method%Pesticide residues%Vegetables
该文研究建立了蔬菜中49种农药的多残留分析方法。前处理采用改进的QuEChERS方法,样品经乙腈提取,氯化钠和无水硫酸镁盐析后,经N-丙基乙二胺(PSA)、C18填料和无水硫酸镁混合型固相分散净化,提取液过滤膜后,用在线GPC/GC-MS-MS在多反应监测模式(MRM)下进行检测和确证。结果表明:49种农药的残留组分在50μg/kg的添加量下,用同种样品基质配制标样进行定量的加标回收率为66%~114%,相对标准偏差为0.4%~16.8%;用相近样品基质配制标样进行定量的加标回收率,除甲胺磷、乙酰甲胺磷、氧化乐果和哒螨灵外,其余的均为60%~117%,相对标准偏差为0.4%~12.7%。该方法具有样品前处理简单、分析时间短、净化效果好等优点,在大批量的蔬菜农药多残留检测领域有很好的应用前景。
該文研究建立瞭蔬菜中49種農藥的多殘留分析方法。前處理採用改進的QuEChERS方法,樣品經乙腈提取,氯化鈉和無水硫痠鎂鹽析後,經N-丙基乙二胺(PSA)、C18填料和無水硫痠鎂混閤型固相分散淨化,提取液過濾膜後,用在線GPC/GC-MS-MS在多反應鑑測模式(MRM)下進行檢測和確證。結果錶明:49種農藥的殘留組分在50μg/kg的添加量下,用同種樣品基質配製標樣進行定量的加標迴收率為66%~114%,相對標準偏差為0.4%~16.8%;用相近樣品基質配製標樣進行定量的加標迴收率,除甲胺燐、乙酰甲胺燐、氧化樂果和噠螨靈外,其餘的均為60%~117%,相對標準偏差為0.4%~12.7%。該方法具有樣品前處理簡單、分析時間短、淨化效果好等優點,在大批量的蔬菜農藥多殘留檢測領域有很好的應用前景。
해문연구건립료소채중49충농약적다잔류분석방법。전처리채용개진적QuEChERS방법,양품경을정제취,록화납화무수류산미염석후,경N-병기을이알(PSA)、C18전료화무수류산미혼합형고상분산정화,제취액과려막후,용재선GPC/GC-MS-MS재다반응감측모식(MRM)하진행검측화학증。결과표명:49충농약적잔류조분재50μg/kg적첨가량하,용동충양품기질배제표양진행정량적가표회수솔위66%~114%,상대표준편차위0.4%~16.8%;용상근양품기질배제표양진행정량적가표회수솔,제갑알린、을선갑알린、양화악과화달만령외,기여적균위60%~117%,상대표준편차위0.4%~12.7%。해방법구유양품전처리간단、분석시간단、정화효과호등우점,재대비량적소채농약다잔류검측영역유흔호적응용전경。
In this study,we established a method for the determination of 49 pesticide residues in vegeta?bles.The samples were pretreated with the improved QuEChERS method,and pesticide residues were extract?ed by acetonitrile,then salted out by NaCl and MgSO4,and followed by the N-propyl ethylenediamine (PSA),C18 packing and anhydrous MgSO4 mixed solid-phase disperse purification,finally the extracts were prepared to be tested and identified using online GPC/GC-MS -MS multiple reaction monitoring mode (MRM)after filtered using 0.22μm membrane.The results showed that the recovery was 66%~114% while the relative standard deviation was 0.4%~16.8% when the 49 kinds of pesticide were added at 50 ug/kg level and prepared with the same solution system.However the recovery was 60%~117% and the relative standard deviation was 0.4%~12.7% when the samples were prepared with the similar solution system ex?cept methamidophos,acephate,omethoate and pyridaben.In a word,the method is simple,easy-pretreating, time-saving,and with high purifying efficiency,so it has good application prospects in the vegetable pesti?cide residues detection area.