气相色谱-串联质谱法测定海藻羊栖菜中的19种有机氯农残

摘要

目的:建立海藻羊栖菜中19种有机氯农药残留分析的气相-质谱联用方法.方法:使用GC-MS法同时检测19种农药残留,色谱系统采用HP-5MS毛细管色谱柱(30 m×0.25 mm,0.25μm);柱温为程序升温,初始温度70℃,保持1 min,以15℃·min-1升温至180℃,再4℃·min-1升温至280℃,保持7 min;进样口温度240℃;采用质谱检测器,电子轰击源EI,离子源温度230℃,采用多反应监测模式.结果:采用所建立的方法对海藻羊栖菜进行检测,对照品与供试品中相邻色谱峰分离情况均良好,除六氯苯外,其他有机氯农残加样回收率均在72%~127%之间,RSD也满足要求.未检出羊栖菜样品中含有有机氯农药残留.结论:方法的建立为海藻类样品有机氯农药残留检测提供了参考.%Objective:To establish a GC-MS method for determing 19 organochlorine pesticide residues in sargassum fusiforme. Methods:Nineteen organochlorine pesticide residues were simultaneously determined by GC-MS, and the established method was vali-dated. The HP-5 gas chromatography column (30 m × 0. 25 mm,0. 25 μm) was used. The column temperature was programming in-creased with initial temperature of 70℃, maintaining for 1min, then raising to 180℃ with a rate of 15℃·min-1 ,and then raised to 280℃ with a rate of 4℃·min-1 to keep 7min. The inlet temperature was 240℃. The MS detector was used with EI source at 230℃, and analysis mode was multiple reaction monitoring. Results:Sargassum fusiforme was analyzed. The separation degree of the standard and samples met the requirements. The recoveries of the organochlorine pesticides were 72%-127% except for hexachlorobenzene, and the relative standard deviation also met the requirements. The experimental results showed that the 19 organochlorine pesticides were not detected out in sargassum fusiforme. Conclusion: The method provides the technical parameters for the determination of organo-chlorine pesticide residues in sargassum fusiforme.