School of Chemical Engineering and Technology, Tianjin University, Tianjin, PR China.
J Sep Sci. 2010 Nov;33(21):3347-53. doi: 10.1002/jssc.201000426.
Ultra performance LC with quadrupole TOF MS (UPLC/Q-TOF-MS) fingerprinting is first developed for the identification of the major components of Phellodendri Amurensis Cortex (PAC). The PAC samples are separated using a Waters ACQUITY UPLC BEH C18 (2.1×50 mm, 1.7 μm) by linear gradient elution using water (containing 0.2% formic acid) and acetonitrile (containing 0.2% formic acid) as the mobile phase. Ten batches of PAC are selected to construct the UPLC/Q-TOF-MS fingerprint. Sixteen common peaks in the fingerprint are obtained, ten of which are tentatively identified, with reference to the literature data, as phellodendrine, magnoflorine, tetrahydropjatrorrhizine, menisperine, tetrahydropalmatine, jatrorrhizine, palmatine, berberine, obacunone, and limonin. Chemometric methods are also employed to evaluate the variation of herbal drugs and other closely related herbs based on the characteristics of peaks in the UPLC/Q-TOF-MS profiles. The developed fingerprint assay is a powerful method that may be used to conduct quality control of PAC.
超高效液相色谱与四极杆飞行时间质谱联用（UPLC/Q-TOF-MS）指纹图谱法首次被开发用于鉴定黄柏（PAC）的主要成分。PAC 样品采用 Waters ACQUITY UPLC BEH C18（2.1×50mm，1.7μm）柱进行分离，采用水（含 0.2%甲酸）和乙腈（含 0.2%甲酸）作为流动相进行线性梯度洗脱。选择十批 PAC 来构建 UPLC/Q-TOF-MS 指纹图谱。从指纹图谱中得到了 16 个共有峰，其中 10 个峰经文献数据参考，被初步鉴定为黄柏碱、木兰碱、延胡索乙素、吴茱萸碱、延胡索甲素、小檗碱、巴马汀、黄连碱、黄柏酮和柠檬苦素。基于 UPLC/Q-TOF-MS 图谱中峰的特征，还采用化学计量学方法来评估草药和其他密切相关草药的变化。所建立的指纹图谱分析方法是一种强大的方法，可用于 PAC 的质量控制。
