Gonzalez Aidee, Foster Krishna L, Hanrahan Grady
Department of Chemistry and Biochemistry, California State University, Los Angeles, CA 90032, USA.
J Chromatogr A. 2007 Oct 12;1167(2):135-42. doi: 10.1016/j.chroma.2007.08.035. Epub 2007 Aug 19.
The successful separation of three benzo[a]pyrene-quinone isomers, two of which were previously unresolved, using liquid chromatography-mass spectrometry (LC-MS) and response surface methodology is presented. Initial efforts centered on chromatographic separation of benzo[a]pyrene-1,6/3,6-quinone peaks evaluated for both resolution and retention time. The mergence of the two parameters was accomplished using the Derringer's desirability function with subsequent optimization by a Box-Behnken response surface design. By implementing the optimal flow rate, column temperature and eluent composition predicted by the validated model, enhanced resolution of the two isomers was achieved in less than 20 min. Calibrations were performed to quantify these isomers and the limits of detection were determined. Optimal model conditions were then used to identify three independent benzo[a]pyrene-quinone isomers produced in the irradiation of a benzo[a]pyrene standard solvated in oxygen-saturated methanol/methylene chloride. This work is not only highly significant to the field of environmental chemistry, but instructive for investigators struggling with the co-elusion of isomeric compounds in their work.
本文介绍了使用液相色谱 - 质谱联用（LC-MS）和响应面方法成功分离三种苯并[a]芘醌异构体，其中两种异构体此前无法分离。最初的工作集中在对苯并[a]芘 - 1,6/3,6 - 醌峰进行色谱分离，并对分离度和保留时间进行评估。通过使用德林格合意函数合并这两个参数，随后采用Box-Behnken响应面设计进行优化。通过实施经过验证的模型预测的最佳流速、柱温和洗脱液组成，在不到20分钟的时间内实现了两种异构体的分离度提高。进行了校准以量化这些异构体，并确定了检测限。然后使用最佳模型条件鉴定了在溶解于氧饱和甲醇/二氯甲烷中的苯并[a]芘标准品辐照过程中产生的三种独立的苯并[a]芘醌异构体。这项工作不仅对环境化学领域具有高度重要意义，而且对在工作中难以分离异构体化合物的研究人员具有指导意义。
