Department of Environmental Science, Aarhus University, Roskilde, Denmark.
Anal Bioanal Chem. 2013 Aug;405(20):6519-27. doi: 10.1007/s00216-013-7100-1. Epub 2013 Jul 6.
A new method for enantioselective analysis of isomers of hexabromocyclododecane (HBCD) is described, using a two-dimensional high-performance liquid chromatography (HPLC) approach to avoid coelution, in particular between (+) α-HBCD, (+) β-HBCD, or (+) γ-HBCD. After isomer separation on a conventional column, the single isomers are transferred to an enantioselective HPLC column using heart cuts. Two enantioseparations are conducted in two separate partial chromatograms: one for α-HBCD and one for β- and γ-HBCD. The result is a completely undisturbed enantioselective separation for α-HBCD at a resolution of 4.11. A peak capacity of 107 was achieved. This peak capacity is utilized by the six peaks of the three isomers with two enantiomers each by 6%. This method was applied to samples of sand eel oil, glaucous gull, and ringed seal. The calibration was performed by treating each enantiomer as a single analyte using a multilevel internal standard calibration. Enantiomeric fractions of 0.495-0.501 with standard deviations (SDs) of 0.056-0.071 were determined for racemic standards of α-HBCD, while the values for fish oil were 0.548-0.562 with SD of 0.018-0.041, depending on the respective mass spectrometric transition.
一种用于对六溴环十二烷（HBCD）异构体进行对映体选择性分析的新方法，使用二维高效液相色谱（HPLC）方法避免共洗脱，特别是（+）α-HBCD、（+）β-HBCD 或（+）γ-HBCD 之间的共洗脱。在常规柱上进行异构体分离后，使用心切割将单一异构体转移到对映体选择性 HPLC 柱上。两种对映体分离在两个单独的部分色谱图中进行：一个用于 α-HBCD，一个用于 β-和 γ-HBCD。结果是在 4.11 的分辨率下对 α-HBCD 进行完全未干扰的对映体选择性分离。实现了 107 的峰容量。这一峰容量由三个异构体的六个峰利用，每个异构体具有两个对映体，利用率为 6%。该方法应用于沙鳗油、银鸥和环斑海豹的样品。通过将每个对映体作为单个分析物使用多级内标校准进行校准。α-HBCD 外消旋标准品的对映体分数为 0.495-0.501，标准偏差（SD）为 0.056-0.071，而鱼油的对映体分数为 0.548-0.562，SD 为 0.018-0.041，具体取决于各自的质谱过渡。
