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目的建立固相萃取-气相色谱-质谱联用(SPE-GC-MS)测定卷心菜粉中联苯菊酯的方法。方法卷心菜粉样品经固相萃取前处理技术进行提取净化。选择乙腈进行超声浸提,经过弗罗里硅土固相萃取柱净化,有效降低了样品基质带来的背景干扰。采用TR-5MS(30 m×0.25 mm,0.25μm)色谱柱程序升温,GC-MS的离子扫描(SIM)模式检测,选择m/z 181、182、166、165作为特征离子,通过外标法定量。结果联苯菊酯浓度为0.03 mg/L~0.90 mg/L时,基质匹配工作曲线线性关系良好,相关系数为0.999 7;在高、低2种浓度添加水平下,方法的平均加标回收率为98.6%~101%,相对标准偏差(RSD)为2.62%~3.08%;该方法的检出限(LOD,S/N=3)为0.006 mg/kg。结论本方法操作简单、快速,重现性较好,灵敏度和准确度均能满足测定卷心菜粉中联苯菊酯的要求。
Objective To establish a method for the determination of bifenthrin in cabbage flour with SPE-GC-MS. Methods Cabbage powder samples were extracted and purified by solid-phase extraction pretreatment. Acetonitrile was selected for ultrasonic extraction and purified by Florisil SPE, which effectively reduced the background interference caused by the sample matrix. The temperature was monitored by TR-5MS (30 m × 0.25 mm, 0.25 μm) column and detected by GC-MS. The m / z 181, 182, 166 and 165 were selected as the characteristic ions. Quantitative. Results When the concentration of bifenthrin was between 0.03 mg / L and 0.90 mg / L, the linearity of the matrix matching curve was good with a correlation coefficient of 0.999 7. The mean spike recoveries The relative standard deviations (RSD) ranged from 2.62% to 3.08%. The limit of detection (LOD, S / N = 3) was 0.006 mg / kg. Conclusion The method is simple, rapid and reproducible. The sensitivity and accuracy of the method are satisfactory for the determination of bifenthrin in cabbage powder.