Department of Chemistry and Biochemistry, Mendel University in Brno, Zemědělská 1, Brno CZ 61300, Czech Republic.
J Chromatogr A. 2012 Mar 30;1231:52-8. doi: 10.1016/j.chroma.2012.02.006. Epub 2012 Feb 9.
The multi-heart-cutting two-dimensional liquid chromatography-tandem mass spectrometry method using atmospheric pressure photoionization has been developed and successfully validated for the determination of nine endocrine disrupting compounds in river water. The method is based on the use of two different reverse-phase columns connected through a six-port two-position switching valve equipped with a 200 μl loop. An orthogonal separation was achieved by proper selection of stationary phases, mobile phases, and the use of a gradient elution in both dimensions. The method shows excellent performance in terms of accuracy (86.2-111.1%), precision (intra-batch: 6.7-11.2%, inter-batch: 7.2-13.5%), and sensitivity (1.2-7.1 ng l(-1)). Twenty real samples collected from the Loučka and the Svratka rivers were analyzed, the studied compounds were found in all Svratka samples (9.7-11.2 ng l(-1) for β-estradiol, 7.6-9.3 ng l(-1) for estrone, and 24.6-38.7 ng l(-1) for bisphenol A).
采用大气压光电离的多切割二维液相色谱-串联质谱法已被开发并成功验证，可用于测定河水中的九种内分泌干扰化合物。该方法基于使用通过配备 200 μl 环的六通二位切换阀连接的两种不同的反相柱。通过适当选择固定相、流动相以及在两个维度上使用梯度洗脱，可以实现正交分离。该方法在准确性（86.2-111.1%）、精密度（批内：6.7-11.2%，批间：7.2-13.5%）和灵敏度（1.2-7.1 ng l(-1)）方面表现出优异的性能。从 Loučka 和 Svratka 河流采集了 20 个实际样品进行分析，在所有 Svratka 样品中都发现了研究的化合物（β-雌二醇为 9.7-11.2 ng l(-1)，雌酮为 7.6-9.3 ng l(-1)，双酚 A 为 24.6-38.7 ng l(-1)）。
