全自动固相萃取分子筛脱水气质联用法测定水中多氯联苯

Determination of Polychlorinated Biphenyls in Water Samples Using Automated Solid Phase Extraction and Molecular Sieve Dehydration Coupled with Gas Chromatography/Mass Spectrometry

建立了气相色谱-质谱联用法测定水中多氯联苯(PCBs)残留的方法。以乙酸乙酯和二氯甲烷为洗脱液,采用C18萃取盘进行全自动固相萃取,萃取液经分子筛脱水后,氮吹浓缩。以PCB209作替代物,菲D10作内标,用选择离子方式进行分析。方法相关系数(R2)为0.9988～0.9999;检出限为1.4×10-6～6.8×10-6mg/L,对实际样品进行加标回收测定(n=3);精密度为0.7%～19.2%;平均加标回收率为80%～115%。本方法具有较好精密度和准确度,前处理方法简单快速,环境友好,可用于工业废水和生活污水中PCBs的测定。

Automated solid phase phy/mass spectrometry （GC/MS） extraction and molecular sieve dehydration coupled with gas ehromatogra- were used to determine the residues of polychlorinated biphenyls （PCBs） in water samples. Using ethylaeetate and dichloromethane as the extraction agent and C8 disk as the extraction disk, extracting liquid was dehydrated by molecular sieve dehydration and concentrated to 1 mL by nitrogen purging. By using PCB209 as a substitute and phenanthrene-D10 as internal standard, selected ion mode was used for the analysis of samples. The proposed method has been applied for the determination of PCBs residues in drinking water and industrial wastewater. The average recoveries were between 80% and 115% with RSD of O. 7%-19.2% （n=3）. The limits of detection was between 1.4x10-6-6.8x10 mg/L and the correlation coefficient of the method （R2 ） was 0. 9988-0. 9999.