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目的建立冷冻干燥-气相色谱法测定干枣中7种拟除虫菊酯类农药。方法试样经冷冻干燥后粉碎,乙腈超声提取,离心,弗罗里硅土柱净化后气相色谱仪直接测定,外标法定量,阳性样品经气相色谱质谱联用法确证。结果加标回收率范围为72.3%~120.1%,相对标准偏差(RSDs)在2.1%~8.1%。将本方法用于实际样品分析,61份干枣中联苯菊酯检出5份,甲氰菊酯检出7份,高效氯氟氰菊酯检出22份,氯氰菊酯检出5份,氰戊菊酯检出6份,氟氯氰菊酯和溴氰菊酯均未检出。结论此方法准确度高,可用于干枣中7种拟除虫菊酯类农药残留的测定。
Objective To establish a method for the determination of seven pyrethroid pesticides in dried dates by freeze-drying-gas chromatography. Methods The samples were freeze-dried and then pulverized. The samples were extracted by acetonitrile, centrifuged and purified by gas chromatography with Florisil column. The external standard method was used for quantification. The positive samples were confirmed by gas chromatography-mass spectrometry. Results The spiked recoveries ranged from 72.3% to 120.1% with relative standard deviations (RSDs) ranging from 2.1% to 8.1%. The method was applied to the actual sample analysis, 61 copies of bifenthrin dried dates were detected 5 copies, 7 fenpropathrin detected, lambda cyhalothrin 22 were detected, cypermethrin 5 copies, cyanide 6 fenvalerate and no cyfluthrin and deltamethrin were detected. Conclusion The method is accurate and can be applied to the determination of seven pyrethroid pesticide residues in dried dates.