建立了分散固相萃取-超高效液相色谱-串联质谱法准确测定城市污水中六溴环十二烷( HBCD)和三-( 2, 3-二溴丙基)异氰脲酸酯( TBC)的方法.对萃取剂用量、萃取时间、淋洗剂、洗脱剂及色谱分离和质谱测定等条件进行了优化.优化后方法为:待测水样加入同位素标记的回收率内标,用0. 4 g Silica、C18和 HLB ( 1:1:1)混合填料分散固相萃取,回收萃取剂后用5 mL的10%的甲醇水溶液淋洗,8 mL甲醇洗脱,氮吹浓缩,加入同位素标记的进样内标测定.方法在1—200 μg·L-1范围线性关系良好,HBCD和TBC的线性相关系数R2>0.9986,检出限为0.6—1.2 ng·L-1 .应用该方法在某大型污水处理厂各工艺段污水中检测出了α-HBCD,浓度水平为1.3—5.4 ng·L-1 .该方法操作简单、灵敏度高,尤其适合城市污水复杂基质中HBCD和TBC的分析.
A method was developed for the analysis of hexabromocyclododecane ( HBCD) and 1,3, 5-Tris ( 2, 3-dibromopropyl ) isocyanurate ( TBC ) in municipal sewage by disperse solid phase extraction ( d-SPE ) and high performance liquid chromatography coupled with tandem mass spectrometry. The amount of extractant, extraction time, lotion and eluent solvent, chromatographic separation method and mass spectrometric determination conditions were optimized. After adding isotope labeled recovery internal standard, water samples were extracted by 0. 4 g mixed filler of silica, C18 and HLB(1:1:1), and the filler was recovered, rinsed with 5 mL of 10% methanol water solution and the targets were eluted by 8 mL of methanol. The elution was concentrated and determined after adding isotope labeled internal standard. Satisfactory method validation results were obtained in linearity (1—200 μg·L-1, R2>0.9986), and the detection limit was in the range of 0.6—1.2 ng·L-1 . The established method was applied to the determination of wastewater from a sewage treatment plant, andα-HBCD was detected in the range of 1.3—5.4 ng·L-1 . The method was simple and efficient, especially suitable for HBCD and TBC analysis in complex matrix samples like municipal sewage.
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