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建立了蔬菜中烯肟菌胺残留量的固相萃取-气相色谱-质谱联用(SPE-GC-MS)分析方法;对烯肟菌胺的裂解机理进行了探讨;确定了测试分析的定性离子和定量离子。样品采用乙酸乙酯高速分散提取,以无水硫酸镁、硅胶和石墨化炭黑(GCB)为混合填料进行固相萃取净化,气相色谱-质谱联用仪在选择离子扫描(SIM)模式下进行检测,基质匹配标准溶液外标法定量。结果显示:烯肟菌胺在0.02~1 mg/L内,标准溶液的峰面积与质量浓度呈良好的线性关系(r>0.999);在0.02~0.2 mg/kg添加水平下,烯肟菌胺的平均回收率为94%~99%,相对标准偏差(RSD,n=6)为2.3%~2.9%;方法的检出限(LOD)(S/N=3)为0.006 mg/kg,定量限(LOQ)(S/N=10)为0.02 mg/kg。
The method of SPE-GC-MS was established for the determination of the residues of ethoxiturine in vegetables. The cleavage mechanism of the insecticides was discussed. The qualitative ions And quantitative ions. The samples were extracted with ethyl acetate at high speed. The samples were purified by solid phase extraction using anhydrous magnesium sulfate, silica gel and graphitized carbon black (GCB) as mixed media. Gas chromatography-mass spectrometry (GC-MS) Detection, matrix matching standard solution of external standard method. The results showed that there was a good linearity (r> 0.999) between the peak area of standard solution and the concentration of standard solution in the range of 0.02 ~ 1 mg / L. When the concentration of netilmicin increased from 0.02 to 0.2 mg / kg, (RSD, n = 6) was 2.3% -2.9%, and the limit of detection (LOD) was 0.006 mg / kg The limit (LOQ) (S / N = 10) was 0.02 mg / kg.