Yu Shengliang, Yang Guipeng, Fu Meng
Key Laboratory of Marine Chemistry Theory and Technology, Ministry of Education, Ocean Chemistry, Ocean University of China, Qingdao 266003, China.
Se Pu. 2007 Jul;25(4):581-5.
A gel permeation chromatographic method was developed for the extraction of 36 pesticides from mushroom prior to gas chromatography with a triple quadrupole mass spectrometric determination. The extraction was based on homogenization with ethyl acetate using a high speed homogenizer. A gel permeation chromatographic clean-up process with ethyl acetate-cyclohexane (1:1, v/v) as mobile phase was applied to the extracts to separate the low-molecular mass pesticides from the high molecular mass compounds in the mushroom. The 7-15 min eluate fraction was collected for subsequent analysis. The target compounds were quantified in the final extract by gas chromatography using a triple quadrupole mass spectrometer with multiple reaction monitoring (MRM). In the linear range (0.01-1.0 mg/L) of each pesticide, the correlation coefficient was higher than 0. 99. The average recoveries (spiked at the levels of 0.01, 0.05, 0.10 mg/kg) were from 72.6% to 117.1% with the relative standard deviations from 2. 0% to 10. 8% (n=5). The limits of detection (LOD) for these pesticides were from 0. 1 to 0.7 microg/kg and the limits of quantification (LOQ) were from 0.2 to 2 Lg/kg.
建立了一种凝胶渗透色谱法，用于在气相色谱-三重四极杆质谱测定之前从蘑菇中提取36种农药。提取基于使用高速匀浆器用乙酸乙酯进行匀浆。采用以乙酸乙酯-环己烷（1:1，v/v）为流动相的凝胶渗透色谱净化过程对提取物进行处理，以将蘑菇中的低分子量农药与高分子量化合物分离。收集7 - 15分钟的洗脱液馏分用于后续分析。使用具有多反应监测（MRM）功能的三重四极杆质谱仪通过气相色谱对最终提取物中的目标化合物进行定量。在每种农药的线性范围（0.01 - 1.0 mg/L）内，相关系数高于0.99。平均回收率（在0.01、0.05、0.10 mg/kg水平加标）为72.6%至117.1%，相对标准偏差为2.0%至10.8%（n = 5）。这些农药的检测限（LOD）为0.1至0.7 μg/kg，定量限（LOQ）为0.2至2 μg/kg。
