气相色谱-串联质谱测定韭菜中的氟氯氰菊酯残留量

Determination of cyfluthrin pesticide residues in leek by gas chromatography-tandem mass spectrometry

中文关键词:  韭菜  氟氯氰菊酯  气相色谱-串联质谱法

英文关键词:leek  cyfluthrin  gas chromatography-tandem mass spectrometry (GC-MS/MS)

中文摘要:

      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×0.25 μm)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。

英文摘要:

      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.