摘要
目的:考察注射用血栓通生产过程关键点及制剂高分子杂质的变化情况,明确去除高分子杂质的关键工艺点。方法:采用凝胶色谱法,色谱柱TSK SWXL2000,7.8 mm×300 mm,6μm,等度洗脱;流动相:乙腈:0.1%三氟乙酸=27∶73;流速:0.5 mL/min;柱温:25℃,检测波长:214 nm。结果:相对分子量对数与保留时间标准曲线r值为0.97,分子量在1638~66430范围内呈良好的线性关系,30批注射用血栓通(冻干)未检测出高分子杂质,三七总皂苷纯化过程步骤C为去除高分子杂质关键步骤。结论:建立的高分子杂质检测方法准确、简便,可作为注射用血栓通制剂及生产过程中间体的内控方法。
Objective: To investigate the key points in the production process of Xueshuantong for injection and the changes of macromolecular impurities in the preparation, and to clarify the key process points for removing macromolecular impurities. Methods: Gel chromatography was performed on the column TSK SWXL2000, 7.8 mm×300 mm, 6 μm, isoocratic elution, mobile phase: acetonitrile: 0.1%trifluoroacetic acid =27∶73;flow rate: 0.5 mL/min;column temperature: 25℃ and the detection wavelength: 214 nm. Results: The r value of the standard curve between the logarithm of relative molecular weight and retention time was 0.97, and the molecular weight showed a good linear relationship in the range of 1638 ~ 66430. No macromolecular impurities were detected in 30 batches of Xueshuantong(lyophilized) for injection, and step C of the purification process of Panax notoginseng saponins was the key step to remove macromolecular impurities. Conclusion: The established method is accurate and simple, and can be used as an internal control method for Xueshuantong preparation for injection and intermediates in the production process.
出处
《大众科技》
2022年第1期35-39,共5页
Popular Science & Technology
基金
广西三七综合利用技术重点实验室,注射用血栓通标准化建设(2YBLH-C-GX-09)。
关键词
凝胶色谱
高分子杂质
生产工艺
gel chromatography
macromolecular impurities
production process
