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目的:分析两面针中拟除虫菊酯类农药残留,为两面针的安全用药及质量控制和标准制定提供科学依据。方法:应用GC-MS法、选择离子监测模式(SIM)对两面针中7种拟除虫菊酯农药残留进行检测。样品经石油醚-丙酮(4∶1,v/v)混合溶剂超声提取,无水硫酸钠-无水硫酸镁-PSA-石墨化碳固相萃取小柱净化,外标法定量,测定两面针中7种拟除虫菊酯类农药残留。结果:应用所建立的色谱方法,可成功地对两面针中7种拟除虫菊酯类农药准确定量和确证。在检测的12批次两面针中,除1号和4号样品含少量的联苯菊酯、8号和9号样品含少量氰戊菊酯和3号、4号、5号样品含少量溴氰菊酯外,其余样品均检测不到7种拟除虫菊酯类农药。结论:12批次两面针样品中7种拟除虫菊酯类农药均未超标。该方法可用于两面针中拟除虫菊酯类微量农药残留的检测,可以推广应用。
OBJECTIVE: To analyze the pyrethroid pesticide residue in two-sided needles and provide a scientific basis for the safe medication, quality control and standard setting of the two-sided needles. Methods: Seven kinds of pyrethroid pesticide residues in two-sided needles were detected by GC-MS and SIM. The samples were extracted with petroleum ether - acetone (4: 1, v / v) mixed solvent and purified by anhydrous sodium sulfate - anhydrous magnesium sulfate - PSA - carbon graphite solid phase extraction cartridges. Seven kinds of pyrethroid pesticide residues. Results: Seven kinds of pyrethroid pesticides were successfully quantified and confirmed by using the established chromatographic method. Among the 12 batches of ampoules examined, samples Nos. 1 and 4 contained a small amount of bifenthrin, samples Nos. 8 and 9 contained a small amount of fenvalerate and Nos. 3 and 4, and sample No. 5 contained a small amount of bromine There were no more than 7 pyrethroid pesticides detected in the rest of the samples. CONCLUSION: Seven pyrethroid pesticides in 12 batches of needle samples did not exceed the standard. The method can be applied to the detection of trace pyrethroid trace residues in the double-sided needles, and can be widely applied.