吹扫捕集-气相色谱-质谱法测定土壤中乙酸乙酯和丙烯酸乙酯

Determination of ethyl acetate and ethyl acrylate in soil by purge and trap gas chromatography-mass spectrometry

建立吹扫捕集-气相色谱-质谱法测定土壤中乙酸乙酯和丙烯酸乙酯的方法。称量5g土壤样品于40mL吹扫瓶中,加入5mL超纯水进行吹扫捕集提取,用DB-624毛细管色谱柱(60m×250μm,1.4μm)分离,全扫描后进行谱库检索定性,内标法定量。乙酸乙酯和丙烯酸乙酯的质量浓度在5.0~200μg/L范围内与定量离子与内标定量离子色谱峰面积的比值线性关系良好,相关系数分别为0.9996和0.9992,检出限分别为1.2、1.4μg/kg。样品加标平均回收率分别为95.8%~108%,79.9%~98.0%,测定结果的相对标准偏差分别为1.92%~13.7%、2.05%~13.8%(n=6)。该方法可用于土壤中乙酸乙酯和丙烯酸乙酯的测定。

A method was developed to determine ethyl acetate and ethyl acrylate in soil by purge and trap gas chromatography-mass spectrometry.A purge bottle of 40 mL was first filled with 5 g soil sample,and 5 mL ultra-pure water was added for purge and trap extraction.DB-624 capillary column(60 m×250μm,1.4μm)was used for separation.Qualitative analysis was then performed through full scan and library searching,and quantitation through internal standard method.The mass concentration of ethyl acetate and ethyl acrylate had a good linear relationship with the ratio of quantitative ion to internal standard quantitative ion chromatography peak area in the range of 5.0-200μg/L,the correlation coefficients were 0.9996 and 0.9992,respectively.The detection limits were 1.2,1.4μg/kg,respectively.The average recoveries of ethyl acetate and ethyl acrylate were 95.8%-108%and 79.9%-98.0%,respectively.The relative standard deviations of the determination results were 1.92%-13.7%and 2.05%-13.8%(n=6),respectively.The method can be used for the detection of ethyl acetate and ethyl acrylate in soil.