高效液相色谱-串联质谱联用法检测母乳中六溴环十二烷异构体  

Determination of hexabromocyclododecanes diastereoisomers in human breast milk by HPLC-MS /MS

作　　者：谭振[1] 陆少游[1] 张建清[1] 蒋友胜[1] 周健[1] 朱舟[1] 刘红河[1] 李胜浓[1] 林晓仕[1] 

机构地区：[1]深圳市疾病预防控制中心,深圳518055

出　　处：《卫生研究》2014年第5期809-813,共5页Journal of Hygiene Research

基　　金：深圳市科技计划重点项目(No.201101016)

摘　　要：目的建立高效液相色谱（HPLC）-串联质谱法（MS/MS）测定母乳中六溴环十二烷三种非对映异构体的方法。方法称取3~5 g冻干母乳样品,加入13C-六溴环十二烷内标,索氏提取,提取液晾干后经6 ml环己烷/乙酸乙酯（1∶1）溶解,凝胶渗透色谱（GPC）除脂,收集液旋转蒸发至近干,加入8 ml正己烷溶解,再加入2 ml浓硫酸进一步除脂,静置分层,收集上清液,正己烷萃取3次,将上清液合并,氮吹至干,定容于100μl甲醇,用HPLC-MS/MS测定。结果方法线性范围为1~50μg/L,相关系数0.9997~0.9998,检出限0.12~0.22μg/L;三个水平的平均加标回收率为82.80%~110.60%;日内相对标准偏差为2.72%~9.02%;日间相对标准偏差为3.49%~5.25%。结论该方法用于测定母乳中六溴环十二烷三种非对映异构体,具有操作简单、基质干扰少、准确可靠的优点,可满足检测需求。Objective A method for the determination of α, β and γ- hexabromocyclododecanes （HBCDs） in human breast milk was developed by HPLC-MS/ MS. Methods 3 -5 g human breast milk powder was spiked with 13C-HBCDs and then been extracted using Soxhlet extraction. The extract was dried and dissolved in 6ml of cyclohexane/ethyl acetate （1：1 ）, then purified by gel permeation chromatography （GPC）. The effluent was concentrated with rotary evaporation and then re-dissolved in hexane. 2 ml of sulphuric acid was added to remove the fat for further clean-up. After drying under nitrogen, the supernatant was dissolved in 100 μl of methanol and finally determined by HPLC-MS/MS. Results The linear range for the three diastereoisomers of HBCDs was in 1 -50 μg/L, with correlation coefficients ranging from 0. 9997 to 0. 9998. The detection limits of the three diastereoisomers ranged from 0. 12 to 0.22 μg/L. The recoveries for three spiking levels ranged from 82.80% to 110.60%. Theintra-day and inter-day relative standard deviations Conclusion The developed method was simple, suitable for the determination of α,βand γ-HBCDs the future. （RSD） were all less than 9.4% convenient and sensitive. It was in breast milk and other matrix in

关 键 词：高效液相色谱串联质谱法 母乳 六溴环十二烷 

分 类 号：R994.4[医药卫生—毒理学]