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目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定韭菜中氯氟氰菊酯残留量的分析方法。方法将韭菜样品的乙腈提取物经石墨化碳黑/氨基混合型固相萃取柱净化、乙腈-甲苯(3:1,V:V)洗脱以及浓缩定容后进行检测。目标化合物经SLB-5MS(30 m×0.25 mm,0.25μm)色谱柱分离后,通过三重串联四级杆多反应监测模式对其进行定性定量分析。结果在添加水平为0.05~0.50mg/L(n=5)时,氯氟氰菊酯的回收率在81.7%~99.1%之间,相对标准差(RSD)在2.5%~8.7%之间。该方法的线性范围为0.05~0.50 mg/L,相关系数r~2>0.990,检出限为0.001 mg/kg,定量限为0.01 mg/kg。结论该方法能满足韭菜中氯氟氰菊酯残留检测的要求。
Objective To establish a method for the determination of cyhalothrin residue in Chinese chives by gas chromatography-tandem mass spectrometry (GC-MS / MS). Methods Acetonitrile extracts of Chinese chive samples were purified by graphite carbon black / amino mixed solid phase extraction (SPE) column, eluted with acetonitrile - toluene (3: 1, V: V) and concentrated. The target compounds were separated by SLB-5MS (30 m × 0.25 mm, 0.25 μm) column, and then were qualitatively and quantitatively analyzed by triple quadrupole multi-reaction monitoring. Results The recoveries of cyhalothrin ranged from 81.7% to 99.1% and the relative standard deviations (RSDs) ranged from 2.5% to 8.7% at the spiked levels of 0.05-0.50 mg / L (n = 5). The linear range of this method was 0.05-0.50 mg / L with a correlation coefficient of r ~ 2> 0.990. The limit of detection was 0.001 mg / kg and the limit of quantification was 0.01 mg / kg. Conclusion The method can meet the detection requirements of cyhalothrin residue in chives.