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【目的】2013—2016年,在北京、天津、河北和山东采集韭菜样品,采用超高效液相色谱-三重四级杆串联质谱法检测甲胺磷、甲拌磷、甲基对硫磷、对硫磷和毒死蜱的残留量,并对其残留安全性进行评价。【方法】韭菜样品用乙腈提取,石墨碳固相萃取小柱净化,超高效反相液相色谱分离,三重四级杆质谱检测,基质匹配标准溶液的外标法定量,在添加浓度为0.01~5.0 mg/kg时,方法的准确度、灵敏度和精密度满足农药残留检测的要求。【结果】甲胺磷的最高检出浓度由70.51 mg/kg降低到0.03 mg/kg,超标率由38.10%降到2.03%;甲拌磷的最高检出浓度由6.45 mg/kg降低到0.04 mg/kg,超标率由23.81%降到1.35%;甲基对硫磷的最高检出浓度由6.62 mg/kg降低到0.13 mg/kg,超标率由25.40%降到2.70%;毒死蜱的最高检出浓度由3.95 mg/kg降低到0.47 mg/kg,超标率由15.87%降到4.73%;对硫磷的最高检出浓度由22.69mg/kg降低到0.03 mg/kg,超标率由15.08%降到1.35%。【结论】上述农药的最高残留检出浓度和超标率大幅降低,但是韭菜中仍能检出少量残留。应加强安全综合防治技术的研发,加强安全用药的宣传和指导,保障韭菜产品安全。
【Objective】 Leek samples were collected in Beijing, Tianjin, Hebei and Shandong from 2013 to 2016. Methamidophos, phorate, and methyl parathion were detected by ultra performance liquid chromatography-triple quadrupole mass spectrometry. Thiophos and chlorpyrifos residues, and evaluate their residual safety. 【Method】 The samples of leeks were extracted with acetonitrile, cleaned up with graphite carbon SPE cartridge, ultra-high performance reversed-phase liquid chromatography, detected by triple quadrupole mass spectrometry and external standard method of matrix matching standard solution. At 5.0 mg / kg, the accuracy, sensitivity and precision of the method met the requirements of pesticide residue testing. 【Result】 The maximum detectable concentration of methamidophos decreased from 70.51 mg / kg to 0.03 mg / kg and the over-standard rate decreased from 38.10% to 2.03%. The maximum detectable concentration of phorate decreased from 6.45 mg / kg to 0.04 mg / kg, the rate of over-standard decreased from 23.81% to 1.35%, the highest detected concentration of parathion decreased from 6.62 mg / kg to 0.13 mg / kg and the over-standard rate decreased from 25.40% to 2.70% The concentration of parathion decreased from 3.95 mg / kg to 0.47 mg / kg and the rate of over-standard decreased from 15.87% to 4.73%. The highest concentration of parathion decreased from 22.69 mg / kg to 0.03 mg / kg, 1.35%. 【Conclusion】 The highest residue concentration and excess rate of the above pesticides were significantly reduced, but a small amount of residue could still be detected in Chinese chives. Should strengthen the comprehensive prevention and control technology research and development, strengthen the publicity and guidance of drug safety, protection of leek product safety.