QuEChERS气相色谱联用法检测马铃薯中4种拟除虫菊酯类农药残留及基质效应的影响

Determination of 4 kinds of pyrethroid pesticides in potato by QuEChERS-based gas chromatography and influence of matrix effects

中文关键词:  QuEChERS  拟除虫菊酯类农残  气相色谱法  基质效应  马铃薯

英文关键词:QuEChERS  pyrethroid pesticide residues  gas chromatography  matrix effect  potato

中文摘要:

      目的 采用QuEChERS前处理结合气相色谱联用技术建立测定马铃薯中4种拟除虫菊酯类(pyrethroid)农药残留的快速高效检测方法。方法 样品粉碎后采用1%乙酸乙腈提取, 无水硫酸镁和氯化钠盐析, 经十八烷基键合硅胶柱(C18)净化, 气相色谱法对样品进行检测, 外标法定量, 提取后样品进行加标实验, 对马铃薯中拟除虫菊酯类农药检测的基质效应评估。结果 马铃薯基质对4种拟除虫菊酯类农药均存在基质增强效应, 增强比为121.12%~143.43%, 4种拟除虫菊酯在马铃薯基质加标水平(20、50、100 μg/kg)的回收率为76.8%~82.5%; 检出限(S/N=3)与定量限分别为2.8~3.7 μg/kg和8.0~10.0 μg/kg, 相对标准偏差小于8.9%。 结论 该方法简单、灵敏度高、净化效果好, 适用于果蔬中拟除虫菊酯的快速检测。

英文摘要:

      Objective To establish a method for determination of 4 kinds of pyrethroid pesticide residues in potatoes by using QuEChERS-gas chromatography. Methods The samples were extracted with 1% acetonitrile acetate after crushing, salted by anhydrous magnesium sulfate and sodium chloride, and purified by octadecyl bonded silica gel column (C18). The samples were detected by gas chromatography and quantified by external standard method. The matrix effect of pyrethroid pesticides in potato was evaluated by adding standard test after extraction. Results There was matrix enhancement effect on 4 kinds of pyrethroid pesticides, and the enhancement ratios were 121.12%~143.43%. The recovery rates of 4 kinds of pyrethroid pesticides in the potato substrate were 76.8%-82.5% (20, 50, 100 μg/kg). The limits of detection (LODs) and limits of quantitation (LOQs) for 4 kinds of pyrethroid pesticides in potatoes were 2.8-3.7 μg/kg and 8.0-10.0 μg/kg, respectively, and the relative standard deviations (RSDs) were less than 8.9%. Conclusion This method is simple, sensitive and has good purification effect, which is suitable for rapid detection of pyrethroid in fruits and vegetables.