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目的建立同时测定植物油中氰虫酰胺、氯虫苯甲酰胺和氟虫酰胺3种邻氨基苯甲二酰胺类杀虫剂残留量的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。方法植物油经环已烷-乙酸乙酯提取后,采用凝胶渗透色谱(gel permeation chromatography,GPC)系统净化,UPLC采用Syncronic C_(18)色谱柱分离,以乙腈和5 mmol/L乙酸铵溶液作为流动相进行梯度洗脱;质谱采用电喷雾正离子源模式和多反应监测模式测定,以外标法定量。结果 3种邻氨基苯甲二酰胺类农药的方法检出限均能达到0.01 mg/kg,在0.01~0.2 mg/L浓度范围内线性关系良好,相关系数r>0.9988,在0.01、0.02和0.1 mg/kg 3个浓度水平进行加标回收,回收率均在72.6%~90.8%范围之间;RSD在2.9%~9.9%之间。结论该方法快速简便、灵敏度高、净化效果好,且显著地缩短了检测时间,可应用于植物油中邻氨基苯甲二酰胺类农药的快速分析。
OBJECTIVE To establish an ultra performance liquid chromatography-tandem mass spectrometry (MS-MS / MS) system for the simultaneous determination of three kinds of anthranilamide insecticide residues in plant oil, including cyromazid, chlorantraniliprole and flubendiamide spectrometry, UPLC-MS / MS) detection method. Methods The plant oil was extracted with cyclohexane-ethyl acetate and purified by gel permeation chromatography (GPC). UPLC was separated on a Syncronic C_ (18) column with acetonitrile and 5 mmol / L ammonium acetate as Mobile phase gradient elution; mass spectrometry electrospray positive ion source mode and multi-reaction monitoring mode determination, external standard method. Results The detection limits of three kinds of anthranilamide pesticides were all 0.01 mg / kg. The linearity was good in the range of 0.01-0.2 mg / L with the correlation coefficient r> 0.9988. The detection limits were 0.01, 0.02 and 0.1 mg / kg. The recovery rates ranged from 72.6% to 90.8%. The RSD ranged from 2.9% to 9.9%. Conclusion The method is rapid, simple, sensitive and has a good purification effect. It can shorten the detection time significantly and can be applied to the rapid analysis of anthranilamide pesticides in vegetable oils.