Dunphy Richard, Burinsky David J
Johnson & Johnson Pharmaceutical Research & Development, LLC, PO Box 300, Raritan, NJ 08869, USA.
J Pharm Biomed Anal. 2003 Apr 1;31(5):905-15. doi: 10.1016/s0731-7085(02)00674-x.
A sensitive, rapid, and specific method for the detection of choline and acetylcholine in a pharmaceutical preparation is described. The method employs a perfluorinated carboxylic acid as ion-pairing reagent, post-column addition of a surface tension reducing agent and mass spectrometric detection using either selected ion monitoring (SIM) or selected reaction monitoring (SRM) modes. The resulting chromatographic performance is comparable or superior to methods reported previously in both quality of the separation and sensitivity when using mass spectral detection, with the added advantage of reduced cycle time. Acetylcholine is easily and rapidly separated from its major decomposition product choline. The method was able to detect acetylcholine and its primary degradation product choline at the 30 fmol level, with an analysis time of less than 6 min.
描述了一种用于检测药物制剂中胆碱和乙酰胆碱的灵敏、快速且特异的方法。该方法采用全氟羧酸作为离子对试剂，柱后添加表面张力降低剂，并使用选择离子监测（SIM）或选择反应监测（SRM）模式进行质谱检测。在使用质谱检测时，所得到的色谱性能在分离质量和灵敏度方面与先前报道的方法相当或更优，且具有缩短循环时间的额外优势。乙酰胆碱能轻松快速地与其主要分解产物胆碱分离。该方法能够在30飞摩尔水平检测乙酰胆碱及其主要降解产物胆碱，分析时间少于6分钟。
