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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(30 m×0.25 mm×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1.0 ml/min,不分流进样,进样1μl;离子监测扫描(SIM)离子源温度230℃,接口温度280℃,电子能量70 eV,溶剂延迟4 min.。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0.989 0~0.999 7,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 To establish a method for the determination of 49 pesticide residues in edible fungi and ginger by solid-phase extraction coupled with gas chromatography-mass spectrometry (GC-MS), and analyze 74 edible mushrooms and 22 ginger samples. Methods Fresh edible fungi and ginger were extracted with acetonitrile and dry edible fungi were extracted with acetone. The extracts were concentrated and purified by solid-phase extraction. The pesticides were separated on a DB-1701 capillary column (30 m × 0.25 mm × 0.25 μm) / MS detection inlet temperature 250 ℃, carrier gas helium, constant flow 1.0 ml / min, splitless injection, injection 1μl; ion monitoring scanning (SIM) ion source temperature of 230 ℃, the interface temperature of 280 ℃, Energy 70 eV, solvent delay 4 min. Results 49 kinds of pesticides showed a good linearity in the range of 0.25-2.00μg / ml with the correlation coefficient (r) of 0.989 0-0.9997. The spiked recoveries at the concentrations of 8 and 80 μg / kg were 66.5 % ~ 143.8%, RSD was 2.2% ~ 10.8%, the detection limit was 0.1 ~ 10.0μg / kg. Conclusion The method is simple, rapid and reliable, which can meet the detection and analysis requirements of 49 kinds of pesticide residues in fresh edible fungi and ginger.