液相色谱-电喷雾离子阱质谱分析土壤中四溴双酚-A

Determination of Tetrabromobisphenol-A in Soil by High Performance Liquid Chromatography-Electrospray Ion Trap Mass Spectrometry

建立了固相萃取-高效液相色谱-电喷雾离子阱质谱(SPE-HPLC-MS-Trap)分析环境土壤样品中四溴双酚-A(Tetrabrom obisphenol-A,TBBP-A)的方法。样品用正己烷索氏提取,用固相萃取C18小柱富集纯化,外标法定量。结果表明:土壤中不同加标浓度(11.9pg/g^11.9ng/g)四溴双酚-A的回收率分别为:(88.9±1.4)%、(98.7±9.9)%、(97.3±10.2)%、(100.6±2.0)%、(97.7±7.4)%和(99.96±4.73)%;不同浓度平行测量的相对标准偏差为0.83%~6.81%。应用建立的方法对环境土壤样品进行了测定,土壤样品中TBBP-A浓度为(25.2±2.7)ng/g(n=4)。

An analytical method for the determination of tetrabromobisphenol-A （4,4＇-isopropylidine-bis （2, 6-dibromophenol）, TBBP-A） in soil samples by high performance liquid chromatography-mass spectrometry with solid phase extraction （SPE-HPLC-MS-Trap） was developed. The quantification was performed with external standard. The recoveries of TBBP-A spiked concentration range of 11.9 pg/g - 11.9 ng/g soil were （88.9±1.4）%, （98.7±9.9）%, （97.3±10.2）%, （100.6±2.0）%, （97.7±7.4）%, （99.96± 4.7） %, respectively. The relative standard deviation was from 0.8% to 6.8%. Environmental soil samples were determined by SPE-HPLC/ESI （ - ） -MS. The concentration of TBBP-A in soil sample was 25.2 ± 2.7 ng/g （n =4）.