LC-MS-MS测定橡胶厂土壤和沉积物中亚乙基硫脲

Determination of Ethylenethiourea in Soil and Sediment of Rubber Factory by High Performance Liquid Chromatography-Mass Spectrometry

建立了橡胶厂土壤和沉积物中亚乙基硫脲残留的超声提取-高效液相色谱-串联质谱检测方法。样品采用75%甲醇水溶液提取,提取液经C18色谱柱(150 mm×2.1 mm,3μm)分离后进入串联质谱仪检测,采用外标法定量。该方法对土壤和沉积物样品检出限为0.005 mg/kg;加标回收率在72.4%~99.0%之间,相对标准偏差(RSD,n=6)在4.1%~6.3%之间;在0.01~1.0 mg/L范围内线性回归系数R^(2)为0.9998。该方法在一定范围内的线性好,回归系数能R>0.999,重复性好,可有效定性定量准确地对土壤鹤沉积物中亚乙基硫脲进行检测。

A method based on ultrasonic extraction along with high performance liquid chromatography-mass spectrometry was developed for the determination of ethylenethiourea residues in soil and sediment of rubber factory.The sample was extracted using 75%methanol aqueous solution.The extracting solution was carried out on C18 column(150 mm×2.1 mm,3μm)into mass spectrometry and quantified using the external standard method.For soil and sediment,the detection limit of this method was 0.005 mg/kg.The recoveries were in the range 72.4%~99.0%with relative standard deviation(RSD)of 4.1%~6.3%(n=6).The linear correlation coefficient(R^(2))was 0.9998 over the concentration range 0.01~1.0 mg/L.This method showed high sensitivity,good reproducibility and qualitative and quantitative accuracy,and could be suitable for the detection of ethylenethiourea residues in soil and sediment.