Qu Liang, Xiao Yao, Jia Zhixin, Wang Zhe, Wang Caihong, Hu Ting, Wu Caisheng, Zhang Jinlan
State Key Laboratory of Bioactive Substance and Function of Natural Medicines, Institute of Materia Medica, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100050, China.
State Key Laboratory of Bioactive Substance and Function of Natural Medicines, Institute of Materia Medica, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100050, China.
J Chromatogr A. 2015 Jun 26;1400:65-73. doi: 10.1016/j.chroma.2015.04.048. Epub 2015 May 2.
Comprehensive two-dimensional liquid chromatography platform (LC×LC) coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS) is developed to separate, identify and relatively determine the chemical constituents of two types of tripterygium glycosides tablets (TGT). The types and relative contents of the constituents discovered in two kinds of TGT tablets were subsequently compared. C8 and C18 column were used for the separation of the first and second dimensional chromatography ((1)D and (2)D) respectively, and an integrated shift and full gradient mode was used in (2)D. Using this LC×LC-QTOF-MS platform, 92 and 132 constituents were detected in TGT preparations from Hubei and Hunan manufacturers respectively (HB-TGT and HN-TGT), most of which belonged to the diterpenoid, triterpenoid and alkaloid families. 50 and 90 compounds were unique in HB-TGT and HN-TGT, respectively, and their relative contents proportion were 52.0% and 54.2% of HB-TGT and HN-TGT, respectively. Furthermore, two TGT tablets could both lead to obvious change in biochemical parameters, oxidative stress related parameters and histopathological status to different degree. In all, the LC×LC-QTOF-MS platform offer a powerful and efficient method for characterizing, identifying and semi-quantifying chemical components in TGT preparations.
开发了一种综合二维液相色谱平台(LC×LC)与四极杆飞行时间(QTOF)质谱(MS)联用的方法,用于分离、鉴定和相对定量两种雷公藤多苷片(TGT)的化学成分。随后比较了两种TGT片中发现的成分类型和相对含量。分别使用C8和C18柱进行第一维和第二维色谱((1)D和(2)D)的分离,(2)D采用积分位移和全梯度模式。利用该LC×LC-QTOF-MS平台,分别在湖北和湖南厂家的TGT制剂(HB-TGT和HN-TGT)中检测到92种和132种成分,其中大部分属于二萜类、三萜类和生物碱类。HB-TGT和HN-TGT分别有50种和90种化合物是独特的,它们的相对含量分别占HB-TGT和HN-TGT的52.0%和54.2%。此外,两种TGT片均能不同程度地导致生化参数、氧化应激相关参数和组织病理学状态的明显变化。总之,LC×LC-QTOF-MS平台为表征、鉴定和半定量TGT制剂中的化学成分提供了一种强大而有效的方法。