摘要
建立了气相色谱-质谱法测定白酒中氨基甲酸甲酯农药残留的分析方法。探讨了白酒样品前处理条件的优化与选择,酒样用Florisil萃取柱净化和环己烷+乙酸乙酯(1+1)洗脱后,采用选择离子监测模式下的GC-EI/MS分析。当酒样的加标浓度为20μg/L、50μg/L和100μg/L时,加标回收率为78.7%～86.2%,相对标准偏差小于8.2%。本方法中氨基甲酸甲酯的检测限为12.5μg/L,线性范围为0.02～2.0μg/mL,样品中氨基甲酸甲酯的最小检出浓度为0.25μg/L。在检测的6种白酒中,有2种检出氨基甲酸甲酯,含量分别为1.8μg/L、28.9μg/L,其余酒样未检出。此分析方法可用于白酒样品中痕量农药残留的分析。
A method for the determination of methyl carbamate pesticide residue in liquor was established by GC-MS. After the optimization of different parameters such as the extraction solvent, liquor samples was cleaned up on a Florisil column by an elution of mixture of cyclohexane and ethyl acetate （1＋1）, and analyzed by gas chromatography-electron ionization mass spectrometry （GC-EI/MS）in the selected ion monitoring mode （SIM）. Recovery studies were performed at 20, 50 and 100μg/L fortification levels for methyl carbamate, and the recoveries ranged from 78.7 % to 86.2 % with relative standard deviations between 7.6 % and 8.2 %. The limit of detection was 12.5 μg/L. The developed method was linear in the range of0.02～2.0μg/mL. The least detection concentration of methyl carbamate was 0.25 μg/L, Methyl carbamate was found in 2 liquor samples. The content was 1.8 μg/L and 28.9 μg/Lo Sucah method has been successfully applied in the determination of pesticide residues in several liquor samples;
出处
《酿酒科技》
北大核心
2008年第6期106-108,共3页
Liquor-Making Science & Technology
基金
四川省科技厅项目资助(NO.05JY029-66)
