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A strategy for establishment of practical identification methods for Chinese patent medicine from systematic multi-component characterization to selective ion monitoring of chemical markers: Shuxiong tablet as a case study

机译:建立从系统的多组分表征到化学标记物选择性离子监测的中成药实用鉴定方法的策略:以蜀xi片为例

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Authentication of Chinese patent medicine (CPM) is more challenging than that of a single herbal medicine due to the increasing complexity in the chemical matrix. A strategy from systematic multi-component characterization to selective ion monitoring of chemical markers (SMC-SIM) is presented and applied to authenticate Shuxiong tablet (SXT) as a case study. First, an ultra-performance liquid chromatography/quadrupole time-of-flight-Fast DDA (UPLC/QTOF-Fast DDA) approach was developed to comprehensively profile and characterize multi-components in SXT. Second, chemical markers were established using a home-made SXT sample. The SIM method for detection of these markers was initially established on an advanced QTOF mass spectrometer, and then transferred onto an easily accessible single quadrupole QDa detector. Third, the UPLC/QDa-SIM method was used to authenticate commercial SXT samples. Consequently, 250 compounds were characterized, and 73 of them were identified by comparison with reference standards. Two UPLC-SIM methods enabling the monitoring of eleven chemical markers (including five saponins for Notoginseng Radix et Rhizoma, two quinochalcone C-glycosides and a flavonoid O-glycoside for Carthami Flos, one phenolic acid and two phthalides for Chuanxiong Rhizoma), were developed on QTOF and QDa, respectively. Twelve batches of commercial SXT samples were identified by the UPLC/QDa-SIM method. Despite the lower sensitivity, the QDa-SIM method by simple sample preparation achieved similar authentication results, and was more easily generalized in practice than the QTOF-SIM method. In conclusion, targeted monitoring of multiple chemical markers was proven as feasible in comprehensive identification of CPM, and the SMC-SIM strategy enabled establishment of practical quality control methods for CPM that contains a complex chemical matrix.
机译:由于化学基质的复杂性越来越高,中成药的认证比单一草药的认证更具挑战性。提出了一种从系统化多组分表征到化学标记物选择性离子监测的策略(SMC-SIM),并将其作为案例研究应用于验证舒雄片(SXT)。首先,开发了一种超高效液相色谱/四极杆飞行时间快速DDA(UPLC / QTOF-快速DDA)方法来全面分析和表征SXT中的多组分。其次,使用自制的SXT样品建立化学标记。用于检测这些标记的SIM方法最初是在高级QTOF质谱仪上建立的,然后转移到易于访问的单四极杆QDa检测器上。第三,UPLC / QDa-SIM方法用于鉴定商业SXT样品。因此,鉴定了250种化合物,并通过与参考标准进行比较鉴定了73种。开发了两种可以监测11种化学标记物的UPLC-SIM方法(包括用于三七的5种皂苷,用于香樟叶的2种喹诺酮C-糖苷和一种类黄酮O-糖苷,用于川xi的1种酚酸和两种邻苯二酚的监测方法。分别在QTOF和QDa上。通过UPLC / QDa-SIM方法鉴定了十二批商业SXT样品。尽管灵敏度较低,但通过简单样品制备的QDa-SIM方法获得了相似的验证结果,并且在实践中比QTOF-SIM方法更容易推广。总之,证明了对多种化学标记物进行有针对性的监测对CPM的全面鉴定是可行的,并且SMC-SIM策略可以为包含复杂化学基质的CPM建立实用的质量控制方法。

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