Shanghai Research Center for Modernization of Traditional Chinese Medicine, National Engineering Laboratory for TCM Standardization Technology, Shanghai Institute of Materia Medica, Chinese Academy of Sciences, Shanghai 201203, China; Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
J Pharm Biomed Anal. 2014 Jan;88:321-30. doi: 10.1016/j.jpba.2013.08.049. Epub 2013 Sep 8.
Kansui radix is a famous poisonous traditional Chinese medicine. However, due to its different types of constituents with broad polarity, a variety of UV absorptions and lack of the reference standards, it was difficult to simultaneously determine the main component in kanui radix. A single, multi-faceted, enhanced strategy, exogenous reference standard - single standard to determine multi-components method (ERS-SSDMC), was proposed. Thirteen major components of kansui radix, including three jatrophane diterpenoids, eight ingenane diterpenoids and two triterpenes, among which there were three pairs of isomers, were simultaneously assayed. A C8 column, packed with 2.7μm core-shell particles, was optimized to separate these constituents in 25min on HPLC instrument detected at a program wavelength. Ethyl benzoate employed as single exogenous reference standard. The method was fully validated with respect to linearity (r(2)>0.9995), LOQs (0.1-0.4μg/mL), precision, accuracy (92-114%, RSD<4.4%) and stability. The robustness of the method was performed by Plackett-Burmantest tests which eight primary chromatographic parameters were investigated. It was found that the two factors, wavelength and flow rate, should be strictly controlled. A total of 75 batches of kansui radix and its three different processing products were successfully analyzed and discriminated by applying the proposed method. This work demonstrates an effective strategy for the SSDMC method making the simultaneous assay of complex multi-component TCM system achievable.
甘遂是一种著名的有毒中药。然而，由于其具有不同类型的组成成分，极性广泛，多种紫外吸收和缺乏参考标准，因此难以同时确定甘遂中的主要成分。提出了一种单一、多方面、增强的策略，即外源性参考标准 - 单标准测定多成分法（ERS-SSDMC）。同时测定了甘遂中的 13 种主要成分，包括三种大戟二萜、八种大戟二萜和两种三萜，其中有三对异构体。使用 C8 柱，填充 2.7μm 核壳颗粒，在 HPLC 仪器上以程序波长在 25min 内优化分离这些成分。苯甲酸乙酯用作单一外源性参考标准。该方法在 0.1-0.4μg/mL 的范围内进行了充分的线性（r(2)>0.9995）、LOQs（检出限）、精密度、准确度（92-114%，RSD<4.4%）和稳定性验证。通过 Plackett-Burman 测试对方法的稳健性进行了研究，考察了八个主要的色谱参数。结果发现，两个因素，波长和流速，应严格控制。应用所提出的方法成功分析和区分了 75 批甘遂及其三种不同的加工产品。这项工作展示了一种有效的 SSDMC 方法策略，使复杂的中药多成分系统的同时测定成为可能。
