全自动固相萃取-气相色谱-三重四级杆质谱法测定地表水中20种半挥发性有机物

Determination of 20 semi-volatile organic compounds in surface water by fully automated solid-phase extraction-gas chromatography-triple quadrupole mass spectrometry

建立全自动固相萃取-气相色谱-三重四级杆质谱联用仪测定地表水中20种半挥发性有机物的分析方法。用全自动固相萃取装置对半挥发性有机污染物进行提取、富集,经DB-5MS色谱柱(30 m×0.25 mm,0.25μm)分离,用全扫描模式定性,以多反应监测(MRM)模式联合内标法定量分析。20种半挥发性有机物的质量浓度在20~1000μg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.9990,方法检出限为0.010~0.023μg/L。样品加标平均回收率为83.5%~103.1%,测定结果的相对标准偏差为0.76%~3.08%(n=6)。该方法既可提高萃取效率,又具有灵敏度高、准确度高等优点,适用于地表水中微量半挥发性有机物的分析。

A method for the determination of 20 semi-volatile organic compounds(SVOCs)in surface water by fully automated solid-phase extraction-gas chromatography-triple quadrupole mass spectrometer was established.SVOCs were extracted and enriched using a fully automated solid-phase extraction device,separated by DB-5MS chromatographic column(30 m×0.25 mm,0.25μm),qualitatively analyzed using full-scan mode,and quantitatively analyzed using multiple reaction monitoring(MRM)mode with internal standard method.The mass concentration of 20 SVOCs had a good linear relationship with the chromatographic peak area in the range of 20-1000μg/L,the correlation coefficients were all more than 0.9990,and the detection limits were 0.010-0.023μg/L.The average recoveries of sample spiked were 83.5%-103.1%,and the relative standard deviations of the determination results were 0.76%-3.08%(n=6).The method can improve extraction efficiency,with high sensitivity and accuracy,which is suitable for the analysis of trace SVOCs in surface water.