气相色谱-串联质谱法测定韭菜中的氯氟氰菊酯残留

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

中文关键词:  韭菜  氯氟氰菊酯  气相色谱-串联质谱法

英文关键词:leek  cyhalothrin  gas chromatography-tandem mass spectrometry

中文摘要:

      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, 0.25 μm)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0.05~0.50 mg/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r2>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。

英文摘要:

      Objective To establish a method for determination of cyhalothrin in leek by gas chromatography- tandem mass spectrometry (GC-MS/MS). Methods The acetonitrile extraction of leek samples was purified by amino hybrid graphitized carbon black/solid phase extraction column, eluted by acetonitrile-toluene (3:1, V:V) and detected after concentration. The target compounds were separated using a SLB-5MS (30 m×0.25 mm, 0.25 μm) chromatographic column, and analyzed qualitatively and quantitatively by triple tandem level 4 pole multiple reaction monitoring mode. Results At addition levels of 0.05~0.50 mg/L (n=5), recovery rates of cyhalothrin were between 81.7%~99.1%, and the relative standard deviations (RSDs) were between 2.5%~8.7%. The linear range of the method was 0.05~0.50 mg/L with the correlation coefficient above 0.99, and the limit of detection and the limits of quantification were 0.001 mg/kg and 0.01 mg/kg, respectively. Conclusion The established method can satisfy the detection requirements of the residue of cyhalothrin in leek.