将气相色谱-负离子化学源/质谱法(gC-nCI/MS)应用于分析海洋生物中五种多溴联苯醚(PbdES)和五种多溴联苯(PbbS)残留。样品以正己烷/丙酮(1∶1,V/V)作为提取剂,采用超声萃取法,提取液经酸性硅胶和中性硅胶层析柱净化和正己烷洗脱后,以PCb-103为内标物和gC-nCI/M的选择离子监测方式(SIM)进行定性与定量分析。平均加标回收率为82.7%~101.0%,相对标准偏差小于5.6%,方法检测限都小于0.20x10-9,PbdES的线性范围是(0.1~500)x10-9,PbbS的线性范围是(0.35~350)x10-9,相关系数都大于0.9999。所分析生物样品中PbdE-47是最主要检出目标物。A rapid method based on ultrasonic extraction was developed for the determination of five polybrominated diphenyl ethers(PBDEs) and five polybromodiphenyls(PBBs) in fish and mussel.Hexane/acetone(1/1) was used as the extraction solvent,and hexane was elution solvent,after the extraction was cleaned by the cartridge filled with silica gel and acidic silica gel,the analysis of samples was accomplished using gas chromatography with negative chemical ionization mass spectrometric detection(GC-NCI/MS) in the selected ion monitoring mode(SIM),and with PCB-103 as internal standard(IS).The average recoveries of the spiked standard samples ranged from 82.7% to 101.0% with a relative standard deviation that was less than 5.6%,and the detection limit of the method was lower than 0.20×10-9 for all PBDEs and PBBs,the range of linearity was from 0.1×10-9 to 500×10-9 for PBDEs,and 0.35×10-9 to 350×10-9 for PBBs,with determination coefficients>0.9999.PBDE-47 was the main in all studied samples
