建立了气相色谱串联质谱法快速测定水体中10种多溴联苯醚(PBDEs)含量的分析方法。使用10%样品体积的二氯甲烷溶液进行液液萃取,重复2次,合并的萃取液经减压浓缩后使用二氯甲烷复溶;采用15 m的DB-5 HT色谱柱分离,在280℃进样口温度、1.8 mL/min氦气流速、320℃离子源与GC接口温度、离子监测模式等条件下进行测定。方法学验证结果表明,10种多溴联苯醚在0.5~150 ng/L质量浓度范围内决定系数R²>0.999 0,检出限在0.14~1.89 ng/L,回收率在84.06%~106.99%,精密度在0.96%~5.43%(n=6)。该方法操作简便快速、灵敏度高、稳定性好,适用于水中10种多溴联苯醚化合物含量的快速测定。实际样品测试结果显示,海水中未检出PBDEs,生活污水及养殖废水中PBDEs含量在0.13~0.35 ng/L。

An analysis method is established for the rapid determination of 10 kinds of polybrominated diphenyl ethers (PBDEs) in water by gas chromatography tandem mass spectrometry.The extraction is carried out by using 10% sample volume of dichloromethane solution,repeated twice,and the combined extracts are concentrated under reduced pressure and re-dissolved with dichloromethane.The separation is performed on a 15 m DB-5 HT chromatographic column,and the determination is conducted under the following conditions:injection port is at 280℃,helium flow rate is 1.8 mL·min^-1,both ion source and GC interface temperature are at 320℃,and ion monitoring mode is selected.Methodological validation shows that the linearities of the 10 kinds of PBDEs range from 0.5-150 ng·L^-1 with a determination coefficient R²>0.999 0.The detection limits range from 0.14-1.89 ng·L^-1,the recoveries range from 84.06%-106.99%,and the precision ranges from 0.96%-5.43% (n=6).This method can be used for the rapid determination of 10 kinds of PBDEs in water with easy and fast operation,high sensitivity and stability.Actual sample test results show that PBDEs are not detected in seawater,while domestic sewage and aquaculture wastewater contain PBDEs in the range of 0.13-0.35 ng·L^-1.

刘磊(1998-),男,硕士,从事国产色谱-三重四极杆质谱应用,通讯联系人,15558009605,936614527@qq.com。