Paik Man-Jeong, Nguyen Duc-Toan, Kim Kyoung-Rae
Biometabolite Analysis Laboratory, College of Pharmacy, Sungkyunkwan University, Suwon 440-746, South Korea.
J Chromatogr A. 2006 Jan 20;1103(1):177-81. doi: 10.1016/j.chroma.2005.11.078. Epub 2005 Dec 19.
Solvent extractive two-phase menthoxycarbonyl (MnOC) derivatization was combined with trimethylsilyl (TMS) reaction for enantioseparation of beta-blockers by gas chromatography employing achiral DB-5 and DB-17 dual-columns of different polarity. beta-Blockers in alkaline solution were vortex-mixed with menthyl chloroformate present in dichloromethane to be extracted as diastereomeric N-MnOC derivatives. The subsequent O(N)-TMS reaction allowed complete enantioseparations of two beta-blockers and partial separations of five as N-MnOC/O(N)-TMS derivatives in a single analysis. The temperature-programmed retention index sets were characteristic of each derivative, facilitating chiral discrimination of each enantiomer.
溶剂萃取两相甲氧基羰基（MnOC）衍生化与三甲基硅烷基（TMS）反应相结合，采用不同极性的非手性DB - 5和DB - 17双柱，通过气相色谱法对β-受体阻滞剂进行对映体分离。碱性溶液中的β-受体阻滞剂与二氯甲烷中的氯甲酸薄荷酯涡旋混合，以提取为非对映体N - MnOC衍生物。随后的O（N）-TMS反应能够在单次分析中实现两种β-受体阻滞剂的完全对映体分离以及五种N - MnOC/O（N）-TMS衍生物的部分分离。程序升温保留指数集是每种衍生物的特征，有助于对每个对映体进行手性鉴别。
