A new method for determination of halogenated flame retardants in human milk using solid-phase extraction.
A new method for determination of halogenated flame retardants in human milk using solid-phase extraction.
复制标题
固相萃取测定母乳中卤代阻燃剂的新方法
DOI：
10.1093/jat/26.3.129
复制
发表时间：
2002
影响因子：
2.5
通讯作者：
G. Becher
中科院分区：
文献类型：
--
作者：
C. Thomsen;H. Leknes;E. Lundanes;G. Becher
建立了一种定量测定母乳中多种卤化阻燃剂的方法。该方法已用于7种多溴二苯醚(PBDEs)、BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154和BDE-183，以及卤代苯酚2，4，6-三溴苯酚(TriBP)、五溴苯酚(PEBP)、四氯双酚-A(TCBP-A)和四溴双酚-A(TBBP-A)。样品制备包括使用N-乙烯基吡咯烷酮-二乙烯基苯共聚物进行固相萃取，柱上脂肪分解，然后在硫酸-硅胶柱上进行额外的净化和酚类化合物的甲基化。以5%苯基95%二甲基聚硅氧烷为色谱柱，采用气相色谱-电子捕获质谱法进行分离检测。该方法已在1.8-180pg/g牛奶范围内对大多数卤代阻燃剂进行了验证。平均绝对回收率为49%~83%，内标平均回收率为53%~121%。所有化合物的估计检出限在0.3至1.0 pg/g牛奶之间，样本量为5 g，但TCBP-A除外，其检测下限估计为6.7 pg/g牛奶。
A method has been developed for quantitation of a selection of halogenated flame retardants in human milk. The method has been validated for seven polybrominated diphenyl ethers (PBDEs), BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, and BDE-183, and the halogenated phenols 2,4,6-tribromophenol (TriBP), pentabromophenol (PeBP), tetrachlorobisphenol-A (TCBP-A), and tetrabromobisphenol-A (TBBP-A). The sample preparation includes solid-phase extraction using an N-vinylpyrrolidone-divinylbenzene copolymer with on-column lipid decomposition followed by additional cleanup on sulfuric acid-silica columns and methylation of the phenolic compounds. Separation and detection were performed by gas chromatography-electron capture mass spectrometry, using a 5% phenyl 95% dimethylpolysiloxane column. The method has been validated in the range of 1.8-180 pg/g milk for most of the halogenated flame retardants. The average absolute recoveries were from 49 to 83%, and the average recoveries with respect to internal standards were in the range of 53 to 121%. Estimated limits of detection were in the range of 0.3 to 1.0 pg/g milk using a sample size of 5 g for all compounds, except TCBP-A, for which the limit of detection was estimated to 6.7 pg/g milk.