超声辅助提取-固相萃取-气相色谱-质谱法测定污泥中12种多环芳烃

GC-MS Determination of 12 PAHs in Sludge with Ultrasonic Assisted Extraction and Solid Phase Extraction

污泥样品(约1g)经30mL的体积比为1∶1的乙酸乙酯和丙酮的混合液超声提取1.0h。离心后,取上清液,用硅固相萃取柱进行净化,采用气相色谱-质谱法测定净化液中12种多环芳烃的含量。在气相色谱分离中采用HP-5MS石英毛细管色谱柱,在质谱分析中采用选择离子监测模式。12种PAHs的质量分数均在5~500μg·kg^-1内与其对应的峰面积呈线性关系,检出限为2.29~14.50μg·kg^-1。以空白污泥样品为基体进行加标回收试验,所得回收率为54.9%~108%,测定值的相对标准偏差(n=7)为0.10%~5.4%。

The sludge sample(about 1 g)was extracted ultrasonically for 1.0 hwith 30 mL of mixed solution of ethyl acetate and acetone with volume ratio of 1∶1.After centrifugation,the supernatant was taken and purified with solid phase extraction column of silicon.GC-MS was applied to the determination of 12 PAHs in the purified liquid.The HP-5 MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass fraction of the 12 PAHs were kept in the same range of 5-500μg·kg^-1,with detection limits in the range of2.29-14.50μg·kg^-1.On the base of blank sludge sample,test for recovery was made by standard addition method;values of recovery found were in the range of 54.9%-108%,with RSDs(n=7)of determined values in the range of 0.10%-5.4%.