QuEChERS-气相色谱-三重四级杆质谱法检测韭菜中6种农药残留

Determination of pesticide residues in Allium tuberosum by QuEChERS-gas chromatography-triple quadrupole mass spectrometry

中文关键词:  QuEChERS  气相色谱-三重四级杆质谱法  韭菜  农药残留

英文关键词:QuEChERS  gas chromatography-triple quadrupole mass spectrometry  Allium tuberosum  pesticide residues

中文摘要:

      目的 建立QuEChERS-气相色谱-三重四级杆质谱法(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)检测韭菜中氧乐果、甲拌磷、毒死蜱、氟虫腈、腐霉利及溴氰菊酯6种农药。方法 结合QuEChERS的前处理, 分别比较了石墨化炭黑柱、C18柱、PSA柱对样品的净化效果, 利用GC-MS/MS进行检测, 外标法进行定量。结果 6种农药在相应的范围内线性关系均良好, 相关系数均在0.99以上, 方法检出限(S/N=3)在0.05~0.85 μg/kg的范围内, 方法定量限(S/N=10)在0.25~2.83 μg/kg的范围内, 在0.05、0.1、0.2、0.5 mg/kg的加标水平下, 6种农药的回收率为87.3%~112.8%, 相对标准偏差为7.6%~16.8%。结论 该方法灵敏、高效、准确度高, 适合韭菜中多数农药残留的快速检测。

英文摘要:

      Objective To establish a method for determination of omethoate, phorate, chlorpyrifos, fipromil, procymidone and deltamethyrin in Allium tuberosum by QuEChERS-gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods After pretreatment of QuEChERS, the purification effects of graphitized carbon black column, C18 column and PSA column were compared. The samples were detected by GC-MS/MS, and the external standard method was used for quantitative analysis. Results The linearities of the 6 pesticides were good in their respective linear ranges with the correlation coefficients higher than 0.99. The limits of detection (S/N=3) were in the range of 0.05-0.85 μg/kg, and the limits of quantation (S/N=10) were in the range of 0.25- 2.83 μg/kg. The average recoveries in different matrices were 87.3%-112.8% with the relative standard devuations of 7.6%-16.8% at the spiked levels of 0.05, 0.1, 0.2 and 0.5 mg/kg. Conclusion The method is sensitive, efficient and accurate, which is suitable for rapid detection of most pesticide residues in Allium tuberosum.