Institute of Microbiology, Academy of Sciences of the Czech Republic, vvi, Vídenská 1083, CZ-142 20 Prague 4, Czech Republic.
Talanta. 2010 Mar 15;80(5):1849-55. doi: 10.1016/j.talanta.2009.10.033. Epub 2009 Oct 24.
A new ultra high-performance liquid chromatography method with UV detection was examined for detection and separation of polychlorinated biphenyls. This included optimization of separation conditions for two model mixtures containing seven and fifteen most relevant congeners, comparison of three types of reversed phase sub-2-micron particle sized columns and assessment of system suitability under the optimized conditions. Calibration curves determined in the range from 0.5 to 50.0 microg/mL exhibited correlation coefficients ranging from 0.997 to 0.999. Lower limits of detection ranged from 0.1 to 0.5 ppm. The most efficient Grace C18 column filled with 1.5 microm particles was then tested to separate the complex commercial mixture Delor 103, where the elution order was confirmed by GC-MS. 13 individual congeners were separated and some of the other co-eluting congeners could be resolved using another separation dimension performed with a mass spectrometry detector. The developed method could be directly applied to the separation of less complex mixtures in aqueous sample matrixes, which are used in general for enzyme degradation studies.
一种新的带有紫外检测的超高效液相色谱法被用于检测和分离多氯联苯。这包括对包含七种和十五种最相关同系物的两种模型混合物的分离条件进行优化，比较三种不同类型的亚 2 微米粒径的反相色谱柱，并在优化条件下评估系统适用性。在 0.5 至 50.0 微克/毫升的范围内测定的校准曲线的相关系数在 0.997 至 0.999 之间。检测限在 0.1 至 0.5ppm 之间。然后，使用填充有 1.5 微米颗粒的高效 Grace C18 柱对复杂的商用混合物 Delor 103 进行测试，通过 GC-MS 确认洗脱顺序。分离出 13 种单体同系物，使用质谱检测器进行另一个分离维度的分析，可解决一些其他共洗脱的同系物。所开发的方法可直接应用于水相样品基质中较简单混合物的分离，通常用于酶降解研究。
