全自动固相萃取-气相色谱质谱法测定饮用水源地水中多氯联苯研究

Determination of Polychlorinated Biphenyls in Drinking Water Source by Automated Solid Phase Extraction and Gas Chromatography/Mass Spectrometry

采用全自动固相萃取-气相色谱质谱法测定饮用水源地水中18种PCBs。于1 L水样中加入10 m L甲醇,用Bond Elut PCB固相萃取小柱对水样进行富集,再分别以8 m L二氯甲烷、乙酸乙酯和二氯甲烷/乙酸乙酯进行洗脱。试验结果表明,在10～300μg/L范围内,18种PCBs线性关系良好,相关系数均在0. 998以上,检出限为0. 52～2. 30 ng/L。当水体中加标浓度为0. 03、0. 10、0. 24μg/L时,平均加标回收率分别70. 4%～83. 2%、77. 7%～88. 2%和81. 8%～94. 1%,相对标准偏差分别为9. 4%～16. 0%、7. 0%～11. 7%和4. 4%～9. 3%。

Methods for determination of18kinds of PCBs in drinking water source by automated solid phase extraction and gas chromatography/mass spectrometry were established and the extractionparameters were optimized.10mL of methanol was added to1L of water and the water samples were enriched with thesolid phase extraction column Bond Elut PCB and eluted with8mL of dichloromethane,ethyl acetate and dichloromethane/ethyl acetate,respectively.The results showed that the linearity of18kinds of PCBs was good in the range of10-300μg/L,the correlation coefficient was above0.998,the detection limit was0.52-2.30ng/L.The average standard recoveries were70.4%-83.2%,77.7%-88.2%and81.8%~94.1%respectively when the spiked concentration was0.03,0.10and0.24μg/L,respectively.The relative standard deviations were9.4%-16.0%,7.0%-11.7%and4.4%-9.3%respectively.