固相萃取-气质联用法测定食用菌与生姜中的多组分农药残留

Determination of multiple pesticide residues in mushroom and ginger by SPE-GC /MS

目的建立一种固相萃取．气相色谱质谱联用法测定食用菌与生姜中的49种农药残留的方法，并对74份食用菌和22份生姜进行了分析测定。方法鲜食用菌和生姜用乙腈提取，干食用菌用丙酮提取，提取液浓缩后采用固相萃取拄净化，DB-1701毛细管柱（30m×0．25mm×0．25μm）对农药进行分离，GC／MS检测进样口温度250℃，载气为氦气，恒流1．0ml／min，不分流进样，进样1斗l；离子监测扫描（SIM）离子源温度230℃，接口温度280℃，电子能量70eV，溶剂延迟4min．。结果49种农药在0．25～2．00μg／ml质量浓度范围内呈良好的线性关系，相关系数（r）为0．9890～0．9997，在8和80μg／kg两个浓度水平的加标回收率为66．5％～143．8％，RSD为2．2％～10．8％，检出限为0．1～10．0μg／kg。结论本方法简单、快速、可靠，能够满足鲜食用菌与生姜中49种农药残留量的检测分析要求。

Objective A method for determination of 49 pesticide residues in mushroom and ginger by SPE-GC/MS was established, and 74 mushroom and 22 ginger samples were detected. Methods The pesticide residues in fresh mushroom and ginger were extracted with acetonitrile, and dry mushroom was extracted with acetone. The extracts were purified by SPE after being concentrated, and DB-1701 capillary column was used for separation. Results There was a good linearity between the peak area and the concentration of 49 pesticide residues within 0. 25 μg/ml -2μg/ml, the correlation coefficients were 0. 989 0 - 0. 999 7, the recoveries of spiked sample at 8 and 80 μg/kg to fresh mushroom and ginger were ranged from 66.5% - 143.8% , RSDs were ranged from 2.2% - 10. 8% , and the detection limits were ranged from 0. 1 - 10.0 μg/kg. Conclusion The method was simple, rapid and reliable. It could be applied to determine pesticide residues in fresh mushroom and ginger.