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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0.05~0.50mg/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R~2>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。
Objective To establish a gas chromatography-tandem mass spectrometry (GC-MS / MS) method for the determination of cyfluthrin in Chinese chives. Methods The samples were extracted with acetonitrile, salted out, cleaned up with carbon black / amino mixed solid phase extraction column and eluted with acetonitrile / toluene (3: 1, v: v). The target compounds were separated on a SLB-5MS (30 m × 0.25 mm × 0.25 μm) column and analyzed by multiple reaction monitoring (MRM) with triple quadrupole mass spectrometry. Results The recoveries of cyfluthrin ranged from 78.5% to 98.0% with relative standard deviations between 3.4% and 8.3% at the level of 0.05-0.50 mg / L (n = 5). The linear range of the method was 0.05-0.50 mg / L with a coefficient of determination R 2> 0.99. The limit of quantification for cyfluthrin was 0.05 mg / kg. , Conclusion The method can meet the detection requirements of cyfluthrin residues in Chinese chives.