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[目的]建立同时检测水果中五氯硝基苯和百菌清残留量的气相色谱-质谱联用(GC-MS)分析方法。[方法]样品经提取净化后,采用内标法进行检测。优化色谱条件,采用选择性离子扫描(SIM)模式进行质谱检测。[结果]在0.10~2.00μg/mL添加水平,2种农药的平均回收率在69.00%~96.15%,相对标准偏差为1.23%~3.60%(n=8)。以信噪比RSN=3计算各农药残留的最低检出限,五氯硝基苯为0.002 mg/kg,百菌清为0.001 mg/kg。[结论]该方法结果准确、重现性好,检出限相对较低,可满足水果中五氯硝基苯和百菌清残留量的检测要求。
[Objective] The research aimed to establish a gas chromatography-mass spectrometry (GC-MS) method for the simultaneous determination of pentachloronitrobenzene and chlorothalonil residues in fruits. [Method] After the sample was extracted and purified, it was detected by internal standard method. Optimize chromatographic conditions using mass spectrometry in selective ion scan (SIM) mode. [Result] The average recoveries of two pesticides ranged from 69.00% to 96.15% with relative standard deviations of 1.23% -3.60% (n = 8) at the level of 0.10-2.00 μg / mL. The minimum detectable limit of each pesticide residue was calculated by RSN = 3, with 0.002 mg / kg for pentachloronitrobenzene and 0.001 mg / kg for chlorothalonil. [Conclusion] The method was accurate, reproducible and the detection limit was relatively low, which could meet the detection requirements of the residues of Pentachlorobenzene and Chlorothalonil in fruits.