Atropisomeric Separation of PCB-95 by HPLC

Prabha Ranasinghe, Christopher I. Olivares, W. Champion, Cindy M Lee
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引用次数: 2

Abstract

2,2’,3,5’,6-Pentachlorobiphenyl (PCB-95) is an environmentally significant chiral PCB, of which enantioselective toxicity, biodegradation and chiral stability studies have been limited to date, as no commercially available enantiomers exist for PCB-95 and due to the lack of an efficient preparatory chiral separation method. A selective, sensitive, and rapid high-performance liquid chromatography with UV detection (HPLC-UV) method has been developed and validated for the chromatographic separation and quantitation of PCB-95 enantiomers. In this study, we resolved enantiomers of PCB-95 using a cellulose tris (4-methylbenzoate) Chiralcel OJ- H column. After evaluating mobile phase compositions and temperatures, optimum separation and detection were obtained with isocratic 100% n-hexane as the mobile phase, a column temperature of 20°C, a flow rate of 1 mL/min, and a detection wavelength of 280 nm. The total run time was 8 minutes. Enantiomer purity was confirmed using enantioselective gas capillary chromatography-electron capture detection. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to limit of detection, limit of quantification, precision, linearity, robustness and ruggedness.
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HPLC法分离PCB-95的atrosom异构
2,2 ',3,5 ',6-五氯联苯(PCB-95)是一种具有重要环境意义的手性多氯联苯,其对映选择性毒性、生物降解和手性稳定性的研究迄今为止受到限制,因为市面上没有可用于PCB-95的对映体,并且由于缺乏有效的准备性手性分离方法。建立了一种选择性、灵敏、快速的高效液相色谱-紫外检测(HPLC-UV)方法,用于PCB-95对映体的色谱分离和定量。在这项研究中,我们使用纤维素三(4-甲基苯甲酸酯)Chiralcel OJ- H柱分离了PCB-95的对映体。通过对流动相组成和温度的评价,确定了以100%正己烷为流动相,柱温为20℃,流速为1 mL/min,检测波长为280 nm的最佳分离检测条件。总运行时间为8分钟。对映体纯度采用对映选择性气相色谱-电子捕获检测法确定。该方法按照国际协调会议(ICH)指南在检测限、定量限、精度、线性、稳健性和耐用性方面进行了验证。
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