摘要
目的建立同时测定心阴片中9个指标性成分(京尼平苷酸、槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷、益母草碱、人参皂苷Rg1、人参皂苷Rb1、黄芪甲苷、毛冬青皂苷甲、麦冬皂苷D、冬青素A)含量的超高效液相-质谱联用方法(UPLC-MS)。方法采用Waters ACQUITY UPLC HSS T3色谱柱(2.1 mm×100mm,1.8μm),0.1%甲酸乙腈-0.1%甲酸水梯度洗脱,体积流量为0.4 mL·min^(-1),柱温为40℃,进样量为2μL。质谱采用电喷雾电离离子源,在负离子模式下检测,扫描范围为m/z 100～1 350。结果京尼平苷酸、槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷、益母草碱、人参皂苷Rg1、人参皂苷Rb1、黄芪甲苷、毛冬青皂苷甲、麦冬皂苷D、冬青素A分别在2.3～2 300.0、1.6～400.0、4.7～1 800.0、2.9～2 300.0、3.3～3 400.0、1.7～200.0、2.2～2 000.0、3.1～200.0、1.9～1 800.0 ng·mL^(-1)范围内的线性关系良好(r>0.999 0);精密度、重复性、稳定性的相对标准偏差(RSD)均小于2.00%;平均加样回收率和RSD分别在97.50%～101.90%和0.81%～2.81%范围内。结论该方法简便、快速、准确,可以为心阴片的质量控制提供参考。
Objective,OβD-glucose-7-O-β-D-gentiobioside,leonurine,ginsenoside Rg1,ginsenoside Rb1,astragaloside IV,ilexsaponin A1,ophiopogonin D and ilexgenin A in Xinyin Tablets. Methods The determination was carried out with a Waters ACQUITY UPLC HSS T3 column(1.8 μm,2.1 mm×100 mm)and the mobile phase comprised of acetonitrile and water containing 0.1% formic acid. The flow rate,column temperature and injection volume were 0.4 mL·min^-1,40 ℃ and 2 μL,respectively. ESI uder negative ion mode with m/z 100~1 350 was used as MS detection conditions.Results The geniposidic acid,quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside,leonurine,ginsenoside Rg1,ginsenoside Rb1,astragaloside IV,ilexsaponin A1,ophiopogonin D and ilexgenin A showed good linearities(r >0.999 0)in the ranges of 2.3-2 300.0,1.6-400.0,4.7-1 800.0,2.9-2 300.0,3.3-3 400.0,1.7-200.0,2.2-2 000.0,3.1-200.0 and 1.9-1 800.0 ng·mL^-1. The RSD of precision,reproducibility and stability were all less than2.00%. The overall recoveries were ranged 97.50-101.90% with the RSD ranging 0.81-2.81%. Conclusion This method is simple,quick and accurate,which can be used for quality control of Xinyin Tablets.
作者
闫翠
凌燕
周政
梁碧容
张璐
王陵军
杨忠奇
冼绍祥
YAN Cui;LING Yan;ZHOU Zheng;LIANG Birong;ZHANG Lu;WANG Lingjun;YANG Zhongqi;XIAN Shaoxiang(First Affiliated Hospital of Guangzhou University of Chinese Medicine, Guangzhou 510405 Guangdong,China)
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2019年第3期370-374,共5页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
国家自然科学基金项目(81673796
81473621
81673920
81373570)
广东省自然科学基金重点项目(2016A030311030)
广州市慢性心力衰竭中医药防治重点实验室项目(201705030006)
