Dynamic Extractions, Ltd., 890 Plymouth Road, Slough, Berkshire, UK.
GlaxoSmithKline, Gunnels Wood Road, Stevenage, Herts, UK.
J Chromatogr A. 2014 Jan 3;1323:49-56. doi: 10.1016/j.chroma.2013.10.089. Epub 2013 Nov 6.
A standardised separation methodology was developed for the purification of crude reaction mixtures containing triphenylphosphine oxide (TPPO) using high performance countercurrent chromatography (HPCCC). A solvent system consisting of hexane/ethyl acetate/methanol/water (5:6:5:6) was used in 1 column volume elution-extrusion mode. The HPCCC methodology was compared with classical RP HPLC purification using a set of 12 representative Mitsunobu reaction mixtures. HPCCC was seen to yield a 65% increase in the average recovery of the target component whilst providing similar final target purities to those obtained by HPLC. By eliminating the need for method development for individual samples, the HPCCC methodology described within provides a simple and efficient means for the purification of the entire family of TPPO-containing reaction products.
采用高效逆流色谱（HPCCC）法，开发了一种从含有三苯基氧化膦（TPPO）的粗反应混合物中分离和纯化的标准方法。采用正己烷/乙酸乙酯/甲醇/水（5:6:5:6）的溶剂体系，在 1 个柱体积洗脱-挤出模式下进行。HPCCC 方法与使用一组 12 个代表性 Mitsunobu 反应混合物的经典反相高效液相色谱（RP HPLC）纯化进行了比较。HPCCC 可使目标成分的平均回收率提高 65%，同时提供与 HPLC 获得的最终目标纯度相当的产物。通过消除对个别样品方法开发的需求，本文描述的 HPCCC 方法为纯化整个 TPPO 反应产物系列提供了一种简单有效的方法。
