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机构地区:[1]上海交通大学医学院附属新华医院,上海200092 [2]上海计划生育科学研究所
出 处:《中国药师》2014年第8期1292-1297,共6页China Pharmacist
基 金:上海市卫生局中医药科研基金(编号:2012G003A);上海市教委优秀青年教师基金(编号:ZZjdyx13092)
摘 要:目的:为了探讨液相色谱-质谱联用(LC-MS)技术在天然产物成分分析中的应用,以黄芩苷、野黄芩苷、汉黄芩素、黄芩素、射干苷、次野鸢尾黄素、芦丁、金丝桃苷等8个黄酮类化合物为研究对象,采用超高压液相色谱-三重四级杆串联质谱分析该8个黄酮类化合物的色谱、质谱特性。方法:色谱柱为ZORBAX SB-C18(2.1 mm×50 mm,1.8μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速为0.3 ml·min-1,柱温为35℃,质谱离子源采用电喷雾离子源(ESI)。结果:8个黄酮化合物在色谱柱上的色谱保留行为与取代羟基及苷化的数目具有相关性,在质谱中野黄芩苷、射干苷、金丝桃苷在负离子模式下具有较好的响应,而黄芩苷、汉黄芩素、黄芩素、次野鸢尾黄素、芦丁在正离子模式下具有较好的响应。苷元的裂解以RDA裂解为主。结论:该8个黄酮化合物的色谱和质谱行为对于未知结构的黄酮化合物的结构解析具有一定的指导意义。Objective: To explore the application of liquid chromatography-mass spectrometry (LC-MS) technology in the rapid iden- tification of components in Chinese herbal medicines and natural products using baicalin, scutellarin, wogonin, baicalein, tectoridin, iris- florentin and rutin as the research objects with high pressure liquid chromatography-triple quadrupole tandem mass spectrometry to analyze the chromatography and mass spectrometry characteristics of the eight flavonoids. Methods: The chromatographic separation was on a ZORBAX SB-CIs (2.1 mmx 50 mm, 1.8 ttm) column with the mobile phase consisting of acetonitrile and water (0. 1% formic acid), the flow rate was 0.3 rnl ~ min i, and the column temperature was 35~C. The mass spectrometry was used with an electrospray ion source. Results: The column chromatographic retention behavior of the eight flavonoids was affected by the number of substituted hydroxyl groups and glycosides. Scutellarin, tectordin and hyperoside had better response to the negative ion mode in the mass spectrum, and the others had better response to the positive ion mode. The primary cleavage mode of aglycone was RDA cleavage. Conclusion: The chromatography and mass spectrometry behavior of the eight flavonoids shows certain guiding significance for the structure analysis of unknown f/avonoid comoounds.
关 键 词:超高压液相色谱-三重四级杆串联质谱 黄酮类化合物 色谱行为 质谱行为
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