摘要
建立了液液萃取耦合气相色谱/质谱联用(GC/MS/MS)分析斑马鱼卵中10种多溴联苯醚(PBDEs),12种甲氧基化多溴联苯醚(MeO-PBDEs)和9种羟基化多溴联苯醚(HO-PBDEs)不同极性组分的同步分析方法。优化了前处理步骤和色谱质谱条件,采用液液萃取法提取目标化合物,不必分离即可实现目标化合物的衍生化,使样品前处理时间大大缩短,实现了不同极性组分化合物的同步分析。采用干法制备酸性硅胶柱纯化,用15 mL正己烷和15 mL二氯甲烷正己烷(1:1,V/V)混合溶剂洗脱效果良好。31种化合物在4.0～500μg/L浓度范周内线性良好,相关系数均大于0.99,回收率在71.6%～133.0%之间;相对标准偏差低于21.5%;检出限在0.09～17.0 ng/g之间。本方法应用到斑马鱼亲子代间转移研究中,对实际样品的检测良好,并发现BDE-47,6-HO-BDE-47,6-MeO-BDE-47,2'-HO BDE-28和2'-MeC-BDE 28可通过母代斑马鱼暴露后,不同程度地转移到子代中。
An analytical method was developed for the simultaneous analysis of 10 kinds of PBDEs,12 MeO-PBDEs and 9 kinds of HO-PBDEs in zebrafish eggs by liquid-liquid extraction coupled with GC/ MS/MS.The conditions of extraction,chromatography and mass spectrometry were optimized.The target compounds were extracted through liquid-liquid extraction and derivatization of HO-PBDEs can be carried out without separation from extraction solution.Thus the pre-treatment time could be shortened and all target compounds could be analyzed simultaneously.Purification was conducted by dry packed acidic silica gel column.All compounds can be eluted with 15mL n-hexane and 15mL of dichloromethane and hexane（1：1,V/V） mixed solvent.Under optimized conditions,31 compounds had good linearity in concentration range from 4.0 to 500μg/L,with correlation coefficient（R^2 ） better than 0.9933,recoveries in the range of 71.6%—133.0%with relative standard deviations less than 21.5%,and the method and instrument detection limits varied from 0.09 to 17.0 ng/g.The presented method was applied for maternal transfer study of BDE-47,6-HOBDE-47, 6-Me（）-BDE-47,2＇-HO-BDE-28 and 2＇-MeO-BDE-28 and turned out to be efficient for real sample analysis.After maternal exposure,the five compounds showed different maternal transfer potency in zebrafish,giving new consideration for the exposure assessment of such compounds.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2012年第11期1698-1702,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金项目(Nos.20977047
20737001)资助
关键词
液液萃取
柱前衍生化
斑马鱼卵
亲子转移
Liquid-liquid extraction
Pre-column derivatization method
Zebrafish eggs
Maternal transfer
