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
2014年
8期
2512-2517
,共6页
张群%刘春华%吴南村%李萍萍
張群%劉春華%吳南村%李萍萍
장군%류춘화%오남촌%리평평
韭菜%氟氯氰菊酯%气相色谱-串联质谱法
韭菜%氟氯氰菊酯%氣相色譜-串聯質譜法
구채%불록청국지%기상색보-천련질보법
leek%cyfluthrin%gas chromatography-tandem mass spectrometry (GC-MS/MS)
目的:建立了韭菜中测定氟氯氰菊酯的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry, GC-MS/MS)分析方法。方法样品用乙腈匀浆提取、盐析、石墨化碳黑/氨基混合型固相萃取柱净化、乙腈/甲苯(3:1, v:v)洗脱,浓缩定容后检测。目标化合物经SLB-5MS(30 m×0.25 mm×0.25μm)色谱柱分离,采用三重串联四级杆多反应监测模式(multiple reaction monitoring, MRM)进行定性定量分析。结果在0.05~0.50 mg/L添加水平时(n=5),氟氯氰菊酯的回收率在78.5%~98.0%之间,相对标准差在3.4%~8.3%之间。方法的线性范围为0.05~0.50 mg/L,决定系数R2>0.99,该方法对氟氯氰菊酯的定量限为0.05 mg/kg。结论该方法能满足韭菜中氟氯氰菊酯残留检测的要求。
目的:建立瞭韭菜中測定氟氯氰菊酯的氣相色譜-串聯質譜(gas chromatography-tandem mass spectrometry, GC-MS/MS)分析方法。方法樣品用乙腈勻漿提取、鹽析、石墨化碳黑/氨基混閤型固相萃取柱淨化、乙腈/甲苯(3:1, v:v)洗脫,濃縮定容後檢測。目標化閤物經SLB-5MS(30 m×0.25 mm×0.25μm)色譜柱分離,採用三重串聯四級桿多反應鑑測模式(multiple reaction monitoring, MRM)進行定性定量分析。結果在0.05~0.50 mg/L添加水平時(n=5),氟氯氰菊酯的迴收率在78.5%~98.0%之間,相對標準差在3.4%~8.3%之間。方法的線性範圍為0.05~0.50 mg/L,決定繫數R2>0.99,該方法對氟氯氰菊酯的定量限為0.05 mg/kg。結論該方法能滿足韭菜中氟氯氰菊酯殘留檢測的要求。
목적:건립료구채중측정불록청국지적기상색보-천련질보(gas chromatography-tandem mass spectrometry, GC-MS/MS)분석방법。방법양품용을정균장제취、염석、석묵화탄흑/안기혼합형고상췌취주정화、을정/갑분(3:1, v:v)세탈,농축정용후검측。목표화합물경SLB-5MS(30 m×0.25 mm×0.25μm)색보주분리,채용삼중천련사급간다반응감측모식(multiple reaction monitoring, MRM)진행정성정량분석。결과재0.05~0.50 mg/L첨가수평시(n=5),불록청국지적회수솔재78.5%~98.0%지간,상대표준차재3.4%~8.3%지간。방법적선성범위위0.05~0.50 mg/L,결정계수R2>0.99,해방법대불록청국지적정량한위0.05 mg/kg。결론해방법능만족구채중불록청국지잔류검측적요구。
Objective An analytic method was established for determination of cyfluthrin in leek by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were extracted with acetonitrile after homogenization. The organic phase was then separated from water phase by adding NaCl and further purified on carbon/NH2 column with elution solvents of acetonitrile/toluene (3:1, v:v). Finally, the organic phase was concentrated and reduced for analysis. The target analytes were separated by capillary gas chromatography column SLB-5MS (30 m×0.25 mm×0.25 μm). A tandem quadrupole spectrometer was used for the qualitative and quantitative analysis of the constituents under multiple reaction monitoring (MRM). Results The average recoveries of three pesticides ranged from 78.5%to 98.0%with relative standard deviations (RSDs) of 3.4%~8.3%at the spiking levels from 0.05 mg/kg to 0.50 mg/kg (n=5). The calibration curve showed a good linearity in the range of 0.05~0.50 mg/L, with the coefficient of determination over 0.99 (R2>0.99). The limit of quantitation (LOQs) was 0.05 mg/kg for cyfluthrin in leek. Conclusion The method is available for the determination of cyfluthrin pesticide residues in leek.