CAJ | 학술논문

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。
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.