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目的:建立一种快速检测人参中33种农药残留的QuEChERS-气相色谱-质谱法(QuEChERS-GCMS)。方法:样品以1%冰醋酸-乙腈提取,经醋酸钠、氯化钠、无水硫酸镁盐析后,上清液加入N-丙基二乙胺(PSA)、石墨碳黑(GCB)进行分散固相萃取净化。结果:33种农药在100~1000 ng·mL~(-1)范围内线性关系良好,相关系数r>0.9969,3个添加水平(100 ng·g~(-1)、400 ng·g~(-1)、1000 ng·g~(-1))的平均回收率在78.94%~108.3%范围内,相对标准偏差RSD>15%,方法检出限(LOD)在5~25 ng·g~(-1)范围内;定量限(LOQ)在10~50 ng·g~(-1)。结论:该方法简便快速,灵敏度高,适合于人参中多种农药残留的测定。
Objective: To establish a QuEChERS-GCMS method for rapid determination of 33 pesticide residues in ginseng. Methods: The samples were extracted with 1% glacial acetic acid - acetonitrile. After salting out with sodium acetate, sodium chloride and anhydrous magnesium sulfate, the supernatant was treated with N - propyl diethylamine (PSA) and graphite carbon black (GCB) Dispersive solid-phase extraction purification. Results: The linear relationship of 33 pesticides in the range of 100-1000 ng · mL -1 was good with the correlation coefficient of r> 0.9969, the levels of 100 ng · g -1 and 400 ng · g -1 The average recovery was in the range of 78.94% -108.3%. The relative standard deviation (RSD) was 15%. The detection limit of detection (LOD) was in the range of 5 ng / g to 25 ng · g -1. (-1). The limit of quantification (LOQ) was in the range of 10 ~ 50 ng · g ~ (-1). Conclusion: The method is simple, rapid and sensitive. It is suitable for the determination of various pesticide residues in ginseng.