母乳中溴代/氯代阻燃剂及其代谢产物的分析检测方法  

Determination of Chlorinated/Brominated Flame Retardants and their Metabolites in Breast Milk

作　　者：贲玉婕[1] 李龙[1] 王文月[1,2] 李兴红[1] 田媛[2] 徐晓白[1] 

机构地区：[1]中国科学院生态环境研究中心,环境化学与毒理学国家重点实验室,北京100085 [2]北京工商大学,北京100048

出　　处：《分析化学》2013年第1期69-75,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.20877092;21177152)资助

摘　　要：建立了低分辨气相色谱-负化学源质谱法(GC/NCI-LRMS)定性与定量检测母乳中的溴代/氯代阻燃剂及其代谢产物的方法。所检测的溴代/氯代阻燃剂及其代谢产物分为中性化合物和羟基化合物两部分。采用RTX-1614(30 m)作为色谱分离柱,在优化的色谱条件下对8种多溴联苯醚PBDEs(包括BDE209)及其甲氧基代谢产物MeO-PBDEs,多种其它阻燃剂及代谢物等中性化合物同时进行了分离检测;采用DB-5(30 m)作为色谱分离柱,在优化的色谱条件下分离检测了9种羟基多溴联苯醚OH-PBDEs。在母乳样本中加入代用标准或内标,经过超声提取、液液萃取、硅胶净化和浓缩定容等预处理后,分别对中性和羟基化合物进行测定。十溴联苯醚、其它多溴联苯醚、甲氧基多溴联苯醚、得克隆及脱氯产物、其它阻燃剂等中性化合物,及羟基多溴联苯醚在两个添加浓度水平的回收率分别为66.5%～75.4%,84.2%～126.4%,60.9%～115.1%,86.7%～104.9%,42.9%～113.8%和64.7%～129.5%;中性化合物的相对标准偏差均小于22%,羟基化合物的相对标准偏差均小于30%。利用本方法对我国电子垃圾拆解区人体母乳中的目标物进行了分析检测,结果可靠。A method was developed for the determination of trace-amount chlorinated/brominated flame retardants and their metabolites in breast milk by gas chromatography combined with mass spectrum in negative chemical ionization mode （GC/NCI-LRMS）. Chlorinated/brominated flame retardants and their metabolites were classified into netural and phenolic fractions. Neutral targets included eight brominated diphenyl ether （BDE） congeners （including BDE-209）, five MeO-BDE congeners and other new flame retardants or the metabolites. Phenolic targets referred to nine OH-BDEs congeners. The efficient separation of various neutral targets was obtained on a 30-m column （RTX-1614） and that of phenolic targets was achieved on a 30-m column （DB-5） in the optimized GC condition. In the extraction and clean-up procedures, before supersonic extracting, surrogate/internal standards were required spiking into breast milk, then the samples were separated into neutral and phenolic fractions by a liquid-liquid extraction methods. The extracts were cleaned- up further to remove other co-extracts by sulfuric acid silica prior to injection. It was noticeable that phenolic fractions required to be further derived by diazomethane before clean-up. The recoveries of decabrominated diphenyl ethers, other polybrominated diphenyl ethers, methoxyl-polybrominated diphenyl ethers, dechlorane plus and dechlorinated products, other flame retardants, hydroxylated polybrominated diphenyl ethers were 66.5%-75.4% , 84.2%-126.4%, 60.9%-115.1% , 86.7%-104.9%, 42.9%-113.8% and 64.7%- 129.5%, respectively. The RSD of neutral targets were all below 22%, and those of the phenolic targets were all below 30%. The method was used for the determination of targets in breast milk collected from an e-waste dismantling area. The results of quality control showed the method was reliable investigation.

关 键 词：溴代氯代阻燃剂 代谢物 母乳 

分 类 号：R114[医药卫生—卫生毒理学]