农产品加工·学刊(下)
農產品加工·學刊(下)
농산품가공·학간(하)
Academic Periodical of Farm Products Processing
2014年
1期
69-72
,共4页
固相萃取%离子扫描%气相色谱-质谱法%农药残留
固相萃取%離子掃描%氣相色譜-質譜法%農藥殘留
고상췌취%리자소묘%기상색보-질보법%농약잔류
solid phase extraction%ion monitoring%gas chromatography-mass spectrometry%pesticide residue
建立固相萃取-气相色谱-质谱(SPE-GC-MS)法测定动物肌肉中314种农药残留的分析方法。样品用乙腈-水溶液均质提取,加盐后继续均质,离心后取部分乙腈提取液过Envi-18和LC-NH2串联柱净化后供气相色谱-质谱仪分析。采用外标定量法,选择离子扫描方式,对前处理条件和仪器参数进行优化,在最优试验条件下进行测试,检出限(S/N≥10)为0.01~0.05 mg/kg,相对标准偏差为4.6%~15.1%,回收率为58.7%~161.2%,其中回收率为70%~120%的目标物占81.2%。
建立固相萃取-氣相色譜-質譜(SPE-GC-MS)法測定動物肌肉中314種農藥殘留的分析方法。樣品用乙腈-水溶液均質提取,加鹽後繼續均質,離心後取部分乙腈提取液過Envi-18和LC-NH2串聯柱淨化後供氣相色譜-質譜儀分析。採用外標定量法,選擇離子掃描方式,對前處理條件和儀器參數進行優化,在最優試驗條件下進行測試,檢齣限(S/N≥10)為0.01~0.05 mg/kg,相對標準偏差為4.6%~15.1%,迴收率為58.7%~161.2%,其中迴收率為70%~120%的目標物佔81.2%。
건립고상췌취-기상색보-질보(SPE-GC-MS)법측정동물기육중314충농약잔류적분석방법。양품용을정-수용액균질제취,가염후계속균질,리심후취부분을정제취액과Envi-18화LC-NH2천련주정화후공기상색보-질보의분석。채용외표정량법,선택리자소묘방식,대전처리조건화의기삼수진행우화,재최우시험조건하진행측시,검출한(S/N≥10)위0.01~0.05 mg/kg,상대표준편차위4.6%~15.1%,회수솔위58.7%~161.2%,기중회수솔위70%~120%적목표물점81.2%。
A solid phase extraction - gas chromatography - mass spectrometry analysis method for variety of pesticide residue in animal muscles has been developed. The samples are extracted homogeneously in acetonitrile - water solution firstly, and continue to homogenize after adding salt into the above solution. And then centrifugation, the clear supernatant is purified (Envi-18 and LC-NH2 column) to be ready for GC-MS analysis which is performed by using selected ion monitoring (SIM) mode. The pretreatment conditions and instrument parameters are optimized in the study, and all factors are discussed deeply. Under optimal conditions, the detection limits of the proposed method (S/N≥10) are found in the ranges of 0.01~0.05 mg/kg, the recoveries are in the ranges of 58.7%~161.2% which contains 81.2% of projects' recoveries being in the ranges of 70%~120%, and the relative standard deviations are 4.6%~15.1%.