气相色谱串联质谱法测定水体中10种多溴联苯醚
Determination of 10 kinds of polybrominated diphenyl ethers in water by gas chromatography tandem mass spectrometry
刘磊 1杨继伟 1李剑 1童文烽 1徐巧 1俞晓峰1
作者信息
- 1. 杭州谱育科技发展有限公司,浙江 杭州 311305
- 折叠
摘要
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 15m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.
Abstract
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.
关键词
液液萃取/气相色谱串联质谱/多溴联苯醚/水体Key words
liquid-liquid extraction/gas chromatography tandem mass spectrometry/polybrominated diphenyl ethers/water引用本文复制引用
出版年
2024
NETL
NSTL
万方数据