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目的建立蘑菇中25种农药残留的在线凝胶渗透色谱-串联三重四极杆气质联用法。方法样品用乙腈超声提取,提取液经Qu ECh ERS小柱净化,氮吹浓缩后经凝胶渗透色谱(GPC)在线净化。采用DB-5MS(30 m×0.25 mm,0.25μm)色谱柱进行气相色谱-质谱(GC-MS)分析,以外标法定量。结果 25种农药在其浓度范围内均呈现良好的线性关系,线性相关系数(r)≥0.998 0,方法的检出限(LOD)为0.000 3 mg/kg~0.003 0 mg/kg,定量限(LOQ)为0.001 mg/kg~0.010 mg/kg。方法的加标回收率为73.1%~114.0%,相对标准偏差(RSD)为2.14%~8.32%。结论该方法的样品前处理简单,分析时间短,灵敏度和精密度均符合农药残留检测技术的要求,适用于食用菌中多种农药残留的检测。
Objective To establish an online gel permeation chromatography-tandem triple quadrupole mass spectrometry for the determination of 25 pesticide residues in mushrooms. Methods The samples were extracted with acetonitrile by ultrasonic extraction. The extracts were purified by Qu ECh ERS cartridge, concentrated by nitrogen and purified by gel permeation chromatography (GPC). Gas chromatography-mass spectrometry (GC-MS) was performed on a DB-5MS (30 m × 0.25 mm, 0.25 μm) column and quantified by external standard method. Results The results showed that all the 25 pesticides showed a good linear relationship in the concentration range. The linear correlation coefficient (r) ≥0.998 0. The limit of detection (LOD) was 0.000 3 mg / kg ~ 0.003 0 mg / kg. LOQ) was 0.001 mg / kg ~ 0.010 mg / kg. The recoveries of the method were 73.1% ~ 114.0% with relative standard deviations (RSDs) of 2.14% ~ 8.32%. Conclusion The method of sample pretreatment is simple, the analysis time is short, the sensitivity and precision are in line with the requirements of pesticide residue detection technology, suitable for the detection of a variety of pesticide residues in edible fungi.