Chen Xialin, Guo Yujie, Hu Yuanjia, Yu Boyang, Qi Jin
Jiangsu Key Lab of TCM Evaluation and Translational Research, China Pharmaceutical University, Nanjing 210009, PR China.
State Key Laboratory of Quality Research in Chinese Medicine, Institute of Chinese Medical Sciences, University of Macau, Macao 999078, PR China.
J Pharm Biomed Anal. 2016 May 30;124:281-287. doi: 10.1016/j.jpba.2016.02.016. Epub 2016 Feb 15.
Salvianolate Lyophilized Injection (SLI), a traditional Chinese medicinal (TCM) preparation which is used to treat stroke, is composed of multiple salvianolic acids from the aqueous extracts of Salvia miltiorrhiza, and includes mainly protocatechualdehyde, rosmarinic acid, salvianolic acid B, salvianolic acid D, salvianolic acid E, diastereomer of salvianolic acid E, salvianolic acid Y, lithospermic acid and diastereomer of lithospermic acid. It is difficult to quantitatively control the quality of SLI using traditional high performance liquid chromatography due to the highly similar structure of these constituents including three pairs of diastereomers and the lack of commercial resources for most of these constituents as standards. Thus, a highly reproducible, fast, accurate and simple (1)H quantitative nuclear magnetic resonance (qNMR) method without the need for calibration curves and complex computation was established by optimizing the solvent system and acquisition parameters to simultaneously determine the nine salvianolic acids and mannitol in SLI. This method was validated and successfully used to determine 10 batches of SLI and the qNMR data were further analyzed with a vector including angle cosine and the partial least squares method for the quality control of SLI. The results indicated that qNMR can be used as a routine method for the quality control of SLI and may have potential in the quantification of diastereomers in other TCM preparations.
注射用丹参多酚酸盐是一种用于治疗中风的中药制剂，由丹参水提取物中的多种丹酚酸组成，主要包括原儿茶醛、迷迭香酸、丹酚酸B、丹酚酸D、丹酚酸E、丹酚酸E的非对映异构体、丹酚酸Y、紫草酸和紫草酸的非对映异构体。由于这些成分结构高度相似，包括三对对映异构体，且大多数成分缺乏作为标准品的商业资源，因此使用传统高效液相色谱法难以对注射用丹参多酚酸盐的质量进行定量控制。因此，通过优化溶剂系统和采集参数，建立了一种无需校准曲线和复杂计算的高重现性、快速、准确且简单的氢定量核磁共振（qNMR）方法，用于同时测定注射用丹参多酚酸盐中的9种丹酚酸和甘露醇。该方法经过验证，并成功用于测定10批注射用丹参多酚酸盐，同时利用包含夹角余弦和偏最小二乘法的向量对qNMR数据进行进一步分析，以实现对注射用丹参多酚酸盐的质量控制。结果表明，qNMR可作为注射用丹参多酚酸盐质量控制的常规方法，并且在其他中药制剂中非对映异构体的定量分析方面可能具有潜力。
