John H, Schlegel W
Klinik und Poliklinik für Geburtschilfe und Frauenheilkunde, Westfälische Wilhelms-Universität Münster, Germany.
J Chromatogr B Biomed Sci Appl. 1997 Sep 26;698(1-2):9-15. doi: 10.1016/s0378-4347(97)00296-x.
An improved reversed-phase HPLC method for the separation and detection of both hemiacetalic 11-hydroxy anomers of thromboxane B2 (TXB2) is described. Water-acetonitrile mixtures have served as mobile phases. By diminishing stepwise the temperature of the chromatographic system from 40 to 0 degrees C, the UV-absorbance profile of TXB2 changed from one broad peak to two clearly separated narrow peaks corresponding to the two anomers existing in equilibrium. Modification of the mobile phase pH from 1.6 to 6.9 (0 degrees C) resulted in different concentration ratios of the anomers. The equilibrium constant and the Gibbs free energy were calculated. The intermediate open aldehyde form of TXB2 is unstable and, therefore, cannot be observed either by HPLC or by 1H NMR measurements.
本文描述了一种改进的反相高效液相色谱法，用于分离和检测血栓素B2（TXB2）的半缩醛11-羟基异头物。水-乙腈混合物用作流动相。通过将色谱系统的温度从40℃逐步降至0℃，TXB2的紫外吸收图谱从一个宽峰变为两个清晰分离的窄峰，分别对应于处于平衡状态的两种异头物。将流动相pH从1.6调节至6.9（0℃）会导致异头物的浓度比不同。计算了平衡常数和吉布斯自由能。TXB2的中间开链醛形式不稳定，因此，无论是通过高效液相色谱法还是通过1H核磁共振测量都无法观察到。
