Lee J, Lho D S, Kim M, Kim K, Kim Y
Doping Control Centre, Korea Institute of Science and Technology, Seoul, Korea.
Rapid Commun Mass Spectrom. 1998;12(17):1150-60. doi: 10.1002/(SICI)1097-0231(19980915)12:17<1150::AID-RCM282>3.0.CO;2-5.
Formation cyclic boronates for beta-blockers, by use of triethylamine (TEA) and pyridine as catalysts, gives more effective product yield. Eleven beta-blockers, formed by cyclic boronation with n-butylboronic acid and TEA, produced higher yields than by on-column thermal reaction and seven beta-blockers were shown to give the highest yields in the phenyl cyclic boronation with pyridine or TEA by on-column thermal and general reaction. The phenyl cyclic boronate of nadolol produced one peak in the chromatogram and the n-butyl cyclic boronate showed two peaks. On-column derivatization and n-butylboronic acid and pyridine was effective in saving analysis time and for convenience, even though some n-butyl cyclic boronates by cyclic boronation with TEA gave a better yield. In n-butyl cyclic boronation with pyridine by on-column thermal reaction the detection limits were 0.1 to 4 ng/microL in urine with a signal-to-noise ratio of 10:1.
通过使用三乙胺（TEA）和吡啶作为催化剂来形成β受体阻滞剂的环状硼酸酯，可得到更有效的产物产率。通过与正丁基硼酸和TEA进行环状硼氢化反应形成的11种β受体阻滞剂，其产率高于柱上热反应，并且通过柱上热反应和常规反应，7种β受体阻滞剂在与吡啶或TEA进行苯基环状硼氢化反应时产率最高。纳多洛尔的苯基环状硼酸酯在色谱图中产生一个峰，而正丁基环状硼酸酯显示两个峰。柱上衍生化以及正丁基硼酸和吡啶在节省分析时间和方便性方面是有效的，尽管一些通过与TEA进行环状硼氢化反应得到的正丁基环状硼酸酯产率更高。在通过柱上热反应与吡啶进行正丁基环状硼氢化反应时，尿液中的检测限为0.1至4 ng/μL，信噪比为10:1。
