两面针中7种拟除虫菊酯农药残留分析

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 residues in the roots of Zanthoxylum nitidum and provide the scientific foundation for medication safety,quality control and standard establishment. Methods: A GC - MS method with selected ion monitoring (SIM) mode was applied to determine pyrethroid pesticide residues in the roots of Zanthoxylum nitidum.The samples were extracted with the mixture solution of petroleum ether – acetone (4∶1,v/v) and ultrasonic vibrations,and the analytical samples were purified by anhydrous sodium sulfate – anhydrous magnesium sulfate – PSA – PestiCarb – phase extraction (SPE) cartridge.The samples were respectively injected into the GC-MS analytical system for simultaneous analysis of the pyrethroid pesticid residues in the roots of Zanthoxylum nitidum,with external standard method. Results: Accurate quantitation and confirmation of seven pyrethroid pesticide residues were obtained by the established GC-MS method.As a result,samples 1 and 4 were detected with small amounts of bifenthrin,samples 8 and 9 with small amounts of fenvalerate,samples 3,4 and 9 with small amounts of deltamethrin.In the rest samples,the seven pyrethroid pesticides were not detected. Conclusion: The test result shows the seven pyrethroids pesticides in the twelve batches of samples do not exceed their standard limits.This method is simple,rapid,sensitive and suitable to detect pyrethroids pesticide residues in the roots of Zanthoxylum nitidum and can be promoted for wide spread application.