超声萃取分离-气相色谱-质谱法测定土壤中的3种酰胺类化合物含量

GC-MS Determination of 3 Amide Compounds in Soil with Separation by Ultrasonic Extraction

采用超声萃取-气相色谱-质谱法测定土壤中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N,N-二甲基丙烯酰胺等3种酰胺类化合物的含量。样品经丙酮超声提取,在气相色谱分离中用DB-624色谱柱为固定相,在质谱分析中采用全扫描和选择离子监测模式。3种酰胺类化合物的质量浓度均在0.05~20.0mg·L^(-1)范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.5~1.5mg·kg^(-1)之间。加标回收率在85.3%~110%之间,测定值的相对标准偏差(n=7)在1.5%~5.3%之间。

GC-MS was applied to the determination of 3 amides, i. e. N, N-dimethylformamide, N, N- dimethylacetamide and N,N-dimethylacylamide in soil. The sample was extracted ultrasonically with acetone. The extract was separated on DB-624 chromatographic column. Modes of full-scanning and selected ion monitoring were adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 3 amides were kept in the same range of 0. 05--20. 0 mg·kg^-1 , with detection limits （3S/N） in the range of 0. 5-- 1.5 mg·kg^-1. Values of recovery found by standard addition method were in the range of 85. 3%-110%, and values of RSD＇s （n=7） were in the range 0f 1.5%--5.3%