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首页> 外文期刊>Journal of Physical Organic Chemistry >Investigation of sorption phenomena by solid phase extraction and liquid chromatography for the determination of some ether derivatives of tetrabromobisphenol A
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Investigation of sorption phenomena by solid phase extraction and liquid chromatography for the determination of some ether derivatives of tetrabromobisphenol A

机译：固相萃取-液相色谱法测定四溴双酚A某些醚衍生物的吸附现象研究

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摘要

Observed sorption and chromatographic behaviour served as a starting point for the examination of four etherderivatives of the flame retardant tetrabromobisphenol A (TBBPA): dihydroxyethyl (DHEE), dimethyl (DMe), diallyl(DAE) and dibromopropyl (DBPE). To date, there is little or no information about these compounds in the scientificliterature. The targets in the present study had calculated log Kaa, values of 6.0-10. A broad range of different types ofsolvents were used in order to elucidate the mechanisms of sorption onto silica (glass) and two solid phase extractioncartridges based on polystyrene divinylbenzene polymers, hydroxylated (Isolute ENV+) and vinylpyrrolidone (OasisHLB) containing units. Also, three chromatographic columns (C18, C8 and dual C18-based, i.e. a polar ligand togetherwith C18 on a silica surface) were evaluated. The following were observed: desorption of the targets from silica surfaceby 1-propanol showed the best results and the yields were further improved by silylation of the surface. Regardless ofthe experimental test conditions applied, the lowest recovery was seen for the DMe derivative, followed by TBBPAitself, which had calculated log Ka, values in between the other targets. A washing solution containing up to 70%methanol could be used without elution of the targets from the solid phase extraction cartridge . The dihydroxethylether derivative of TBBPA is most probably not affected by environmental relevant pH due to a likely high pKa (ca 15).Also, this study shows that the polar character of the dual-phase column was not as pronounced as asserted by themanufacturer.
机译：观察到的吸附和色谱行为是检查阻燃四溴双酚A（TBBPA）的四种醚衍生物的起点：二羟乙基（DHEE），二甲基（DMe），二烯丙基（DAE）和二溴丙基（DBPE）。迄今为止，科学文献中关于这些化合物的信息很少或没有。本研究中的目标已计算出log Kaa，值为6.0-10。为了阐明在二氧化硅（玻璃）上的吸附机理以及两种基于聚苯乙烯二乙烯基苯聚合物，羟基化（Isolute ENV +）和乙烯基吡咯烷酮（OasisHLB）的固相萃取柱的吸附机理，使用了多种不同类型的溶剂。另外，评估了三个色谱柱（C18，C8和基于双C18的色谱柱，即在硅胶表面上的极性配体以及C18）。观察到以下结果：用1-丙醇将目标物从二氧化硅表面解吸显示出最佳结果，并且通过表面的甲硅烷基化进一步提高了产率。无论采用何种实验测试条件，DMe衍生物的回收率最低，其后是TBBPAitself，其计算出的log Ka值介于其他目标之间。可以使用含有多达70％甲醇的洗涤溶液，而无需从固相萃取柱上洗脱目标物。由于可能存在较高的pKa（ca 15），TBBPA的二羟乙基醚衍生物很可能不受环境相关pH值的影响。此外，这项研究表明，双相色谱柱的极性特征不如制造商所声称的那么明显。

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