UPLC-MS/MS法同时测定金锁固精丸中10种黄酮类成分

Simultaneous Determination of 10 Flavonoids in Jinsuo Gujing Pill by UPLC-MS/MS

目的:建立超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定金锁固精丸中10种黄酮类成分(毛蕊异黄酮葡萄糖苷、杨梅素-3-O-β-D-葡萄糖苷、沙苑子苷A、异槲皮苷、鼠李柠檬素-3-O-β-D-葡萄糖苷、沙苑子苷B、芦丁、金丝桃苷、儿茶素、紫云英苷)的含量。方法:超高效液相色谱采用Waters ACQUITY UPLC BEH C18柱(100 mm×2.1 mm,1.7μm);流动相为甲醇-0.1%甲酸水溶液,梯度洗脱;流速0.2 m L/min;柱温40℃。质谱条件采用电喷雾离子源负离子模式进行检测,多反应监测模式定量测定。结果:在考察的浓度范围内,10种黄酮成分均呈良好的线性关系(r≥0.99951);回收率和RSD为95.34%~107.36%和0.81%~2.64%。结论:该方法可行,重现性好,可为金锁固精丸的质量控制提供参考。

Objective:To develop a determination method of 10 compounds(calycosin-7-O-β-D-glucoside,myricetin-3-O-β-Dglucoside,astragaloside A,isoquercitrin,rhammelin-3-O-β-D-glucoside,astragaloside B,rutin,hyperoside,catechin,astragalin)in Jinsuo Gujing Pill by using UPLC-MS/MS.Methods:UPLC assay was carried out by using Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)with constant temperature of 40℃.The mobile phase consisted of methanol and 0.1%aqueous formic acid in gradient elution at a flow rate of 0.2 mL/min.The mass spectrometric was detected by the electrospray ion source negative ion mode.The multiple reaction monitoring mode was used for quantitative determination.Results:Satisfactory linearity wasachieved with wide linear range and fine determination coefficient(r≥0.99951),the overall recoveries wereranged from 95.34%~107.36%with the RSD ranging from 0.81%~2.64%.Conclusion:The method was feasible and reproducible which could be used for the quality control of Jinsuo Gujing Pill.