Objective Establishing a fingerprint method to identify the characteristic chemicals in the roots of Gentiana macrophylla and evaluate their quality. Methods RP-HPLC was developed for fingerprint analysis and determin...Objective Establishing a fingerprint method to identify the characteristic chemicals in the roots of Gentiana macrophylla and evaluate their quality. Methods RP-HPLC was developed for fingerprint analysis and determination of four ingredients in G. macrophylla roots from different sources. LC-ESI-TOF-MS was employed to identify the chromatographic peaks of the fingerprint. Results Five common peaks were identified by comparing their retention time with reference secoiridoid glucosides. Eight major peaks in chromatographic fingerprint were analyzed by on-line LC-ESI-TOF-MS. Four secoiridoid glucosides were identified based on their MS data. Conclusion The method is specific and could be served for the quality identification and comprehensive evaluation of G. macrophylla.展开更多
目的:基于二维高效液相色谱-四极杆-飞行时间串联质谱技术(2D-LC-Q TOF/MS),鉴定喷昔洛韦乳膏有关物质的结构。方法:采用ODS(250 mm×4.6 mm, 5μm)色谱柱,以0.15%甲酸10 mmol·L^(-1)甲酸铵缓冲溶液-乙腈为流动相,进行一维梯...目的:基于二维高效液相色谱-四极杆-飞行时间串联质谱技术(2D-LC-Q TOF/MS),鉴定喷昔洛韦乳膏有关物质的结构。方法:采用ODS(250 mm×4.6 mm, 5μm)色谱柱,以0.15%甲酸10 mmol·L^(-1)甲酸铵缓冲溶液-乙腈为流动相,进行一维梯度洗脱,对喷昔洛韦乳膏及其依照ICH原则强制降解样品的有关物质进行分离,并分别富集各有关物质;再采用Phenomenex Luna SCX(250 mm×4.6 mm, 5μm)色谱柱,以0.1%甲酸20 mmol·L^(-1)甲酸铵缓冲溶液-乙腈为流动相,进行二维梯度洗脱,实现各有关物质与喷昔洛韦乳膏基质的良好分离。利用电喷雾正离子化-四极杆-飞行时间串联质谱高分辨测定各有关物质母离子及其子离子的准确质量和元素组成,并解析鉴定其结构。结果:在所建立的2D-LC-Q TOF/MS分析条件下,喷昔洛韦与其有关物质分离良好,检测出喷昔洛韦乳膏及其强制降解样品中21个主要有关物质。根据其色谱保留行为、光谱特征、质谱特征及与其他核苷类药物已知有关物质的差异,结合合成和制剂工艺路线分析,可鉴定出它们的结构,它们均为首次被鉴定出的有关物质。结论:研究结果为喷昔洛韦乳膏的质量控制提供了参考依据。展开更多
基金National Science and Technology Ministry "Significant new drugs creation" special science and Technology Major (20082X09101-016)
文摘Objective Establishing a fingerprint method to identify the characteristic chemicals in the roots of Gentiana macrophylla and evaluate their quality. Methods RP-HPLC was developed for fingerprint analysis and determination of four ingredients in G. macrophylla roots from different sources. LC-ESI-TOF-MS was employed to identify the chromatographic peaks of the fingerprint. Results Five common peaks were identified by comparing their retention time with reference secoiridoid glucosides. Eight major peaks in chromatographic fingerprint were analyzed by on-line LC-ESI-TOF-MS. Four secoiridoid glucosides were identified based on their MS data. Conclusion The method is specific and could be served for the quality identification and comprehensive evaluation of G. macrophylla.
文摘目的:基于二维高效液相色谱-四极杆-飞行时间串联质谱技术(2D-LC-Q TOF/MS),鉴定喷昔洛韦乳膏有关物质的结构。方法:采用ODS(250 mm×4.6 mm, 5μm)色谱柱,以0.15%甲酸10 mmol·L^(-1)甲酸铵缓冲溶液-乙腈为流动相,进行一维梯度洗脱,对喷昔洛韦乳膏及其依照ICH原则强制降解样品的有关物质进行分离,并分别富集各有关物质;再采用Phenomenex Luna SCX(250 mm×4.6 mm, 5μm)色谱柱,以0.1%甲酸20 mmol·L^(-1)甲酸铵缓冲溶液-乙腈为流动相,进行二维梯度洗脱,实现各有关物质与喷昔洛韦乳膏基质的良好分离。利用电喷雾正离子化-四极杆-飞行时间串联质谱高分辨测定各有关物质母离子及其子离子的准确质量和元素组成,并解析鉴定其结构。结果:在所建立的2D-LC-Q TOF/MS分析条件下,喷昔洛韦与其有关物质分离良好,检测出喷昔洛韦乳膏及其强制降解样品中21个主要有关物质。根据其色谱保留行为、光谱特征、质谱特征及与其他核苷类药物已知有关物质的差异,结合合成和制剂工艺路线分析,可鉴定出它们的结构,它们均为首次被鉴定出的有关物质。结论:研究结果为喷昔洛韦乳膏的质量控制提供了参考依据。
