气相色谱-电子轰击源质谱测定海产品中多溴联苯(醚)  

Determination of polybrominated biphenyls and polybrominated diphenyl ethers in sea food with gas chromatography-electron ionization/mass spectrometry method

作　　者：王俊平[1] 姜小梅[1] 王硕[1] 丰帆[1] 赵云襄[1] 

机构地区：[1]食品营养与安全教育部重点实验室,天津科技大学食品工程与生物技术学院,天津300457

出　　处：《食品工业科技》2011年第3期390-393,共4页Science and Technology of Food Industry

基　　金：国家自然科学基金项目(30571532)

摘　　要：海产品中多溴联苯残留现在已经成为新的食品安全危害因子,但是针对海产品中多溴联苯检测方法的研究还不多。针对海产品基质的特殊性,研究建立了样品的加速溶剂萃取仪(ASE)提取、多层硅胶层析柱净化前处理方法,采用定性离子和外标定量法建立了气相色谱-电子轰击源质谱(GC-EI/MS)法检测海产品中多溴联苯(PBBs)和多溴联苯醚(PBDEs)的定性和定量方法。所建立的十三种多溴联苯和多溴联苯醚GC-EI/MS方法的线性范围在10～200ng/mL,检出限在0.44～6.0ng/mL之间,具有较宽的线性范围和很高的灵敏度。通过添加回收实验表明,方法回收率在59.7%～97.2%之间,相对标准偏差(RSD)在1.0%～13.7%之间。The aim of this study is to build a method of determining PBBs and PBDEs in sea food with GC-EI/MS method.The samples were extracted with ASE,cleaned up and separated by concentrated sulfuric acid and multilayer silica column. The external standard quantification was used and gained the optimum condition of preparation of samples,and the best condition of Gas Chromatography（ GC） and Mass Spectrometry（ MS） .Also, the requirements of quality,quantity and experimental condition were assessed and the method detection limits were between 0.44ng /mL-1 and 6.0ng /mL-1 .According to the validation of the quality control（ QC） ,the results proved that the analytical method satisfied the requirements of the determination of PBBs and PBDEs in sea food. The recoveries were between 59.7% and 97.2%,of which the relative standard deviations were between 1.0% and 13.7%.

关 键 词：多溴联苯 多溴联苯醚 GC-EI/MS ASE 

分 类 号：TS207.3[轻工技术与工程—食品科学]