论文部分内容阅读
目的:采用GC-ECD法建立5种药材中包括21种有机氯和5种拟除虫菊酯类在内的26种农药残留量的同时测定方法。方法:采用弗罗里硅土固相萃取净化样品,GC-ECD测定,HP-5弹性石英毛细管柱程序升温分离,载气为高纯 N2,柱流量1.0 mL·min-1,恒流方式控制气流,进样口温度260 oC, ECD温度330 oC。结果:弗罗里硅土固相萃取能有效净化药材样品中杂质,26种农药检测限为0.386~2.500 ng·g-1,定量限为 0.879~6.250 ng·g-1, 平均回收率为69.61%~112.80% (RSD=2.43%~15.18%,n=9)。结论:所建立的方法能同时测定 5 种药材中 26 种农药残留量, 可被参照应用于其它类似药材中的农药残留量检测。
OBJECTIVE: To establish a method for simultaneous determination of 26 pesticide residues in 21 medicinal materials including 21 organochlorines and 5 pyrethroids by GC-ECD. Methods: The sample was purified by Florisil solid-phase extraction (SPE-GC) and determined by GC-ECD. HP-5 flexible silica capillary column was used to separate and purify the sample. The carrier gas was high purity N2. The column flow was 1.0 mL · min- Airflow, inlet temperature 260 oC, ECD temperature 330 oC. Results: Florisil SPE could effectively purify the impurities of medicinal samples. The detection limits of the 26 pesticides were 0.386-2.500 ng · g-1, with the limits of quantification of 0.879-6.250 ng · g-1 and the average recoveries of 69.61 % ~ 112.80% (RSD = 2.43% ~ 15.18%, n = 9). Conclusion: The established method can simultaneously determine 26 kinds of pesticide residues in 5 kinds of medicinal herbs, and can be applied to the detection of pesticide residues in other similar medicinal materials.