微波辅助萃取-气相色谱质谱法检测生物体内的多溴联苯醚

建立了微波辅助萃取-气相色谱质谱法测定生物样品中的多溴联苯醚(PBDEs)的方法,优化了萃取剂的种类、萃取剂用量、萃取时间等微波萃取条件和GC-MS仪器分析条件。正己烷-丙酮混合溶剂提取后,经实验室自制的多层硅胶柱分离纯化,用气相色谱-质谱进行测定,该方法基质加标回收率在60%～77%之间,相对标准偏差在11%～18%之间,方法的检测限为0.03～0.20ng/g,适用于生物样品中PBDEs的测定。

Determination of polybrominated diphenyl ethers in biota by microwave-assisted extraction and gas chromatography-mass spectrometry

A rapid method for the determination of PBDEs in biota was developed based on gas chromatography-mass spectrometry after microwave-assisted extraction. The experimental conditions of extraction and determination were optimized. Mixture of hexane and acetone (1∶1) was used as the extraction solvent. The laboratory-made silica gel cartridge was used to clean the extract after the extraction. Determination of sample was accomplished using gas chromatography with electron ionization mass spectrometric detection in the selected ion monitoring mode (SIM). The average recoveries of the standard samples spiked ranged from 60% to 77% with relative standard deviations between 11% and 18%, and the detection limits of the method were between 0.03 and 0.20 ng/g. The method is suitable for the determination of PBDEs in biota.