摘要
目的对生脉饮中麦冬的质量和真伪进行评价,建立测定麦冬高异黄酮A、山麦冬皂苷B和短葶山麦冬皂苷C 3种特征成分的超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)法,为药品监管提供技术支持。方法采用Phenomenex Kinetex F5 C18柱(100 mm×3.0 mm,2.6μm),以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相,梯度洗脱,流速为0.4 mL/min,柱温为30℃,进样量为1μL;采用质谱检测仪、电喷雾正离子及负离子模式、多反应监测进行测定。结果麦冬高异黄酮A、山麦冬皂苷B和短葶山麦冬皂苷C的线性范围分别为0.0167~1.6660、0.0397~15.8720、0.0225~8.9880ng(r≥0.9999),平均回收率分别为85.16%、86.95%、95.07%,RSD分别为2.65%、1.45%、1.14%(n=6)。38批样品中麦冬高异黄酮A含量相差较大,有7批检出山麦冬皂苷B或短葶山麦冬皂苷C。结论该方法简便、灵敏,可用于生脉饮中3种特征成分的检测,为生脉饮中麦冬的质量控制提供参考。
Objective To evaluate the quality and authenticity of Ophiopogon japonicus in Shengmaiyin,establish ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)for the determination of three characteristic components(methylophiopogonanone A,liriopeside B and liriope muscari baily saponin C),and provide technical support for drug supervision.Methods Samples were analyzed on a Phenomenex Kinetex F5 C18 column(100 mm×3.0 mm,2.6μm)in a gradient elution mode with 0.1%formic acid water and-0.1%formic acid acetonitrile as the mobile phase at a flow rate of 0.4 mL/min,the column temperature was 30℃,and the injection volume was 1μL.Mass spectrometer detector,electro spray ion source of positive and negative ions,and multi-reaction monitoring mode were used.Results The linear ranges of methylophiopogonanone A,liriopeside B and liriope muscari baily saponin C were 0.0167-1.6660,0.0397-15.8720 and 0.0225~8.9880 ng(r≥0.9999),respectively.The average recovery rates of these three components were 85.16%,86.95%and 95.07%,respectively,with RSDs of 2.65%,1.45%and 1.14%(n=6).The content of methylophiopogonanone A in thirty-eight batches was quite different.Seven batches of liriopeside B or liriope muscari baily saponin C were detected.Conclusion The method is simple and sensitive,and suitable for determining of three characteristic components in Shengmaiyin,which provides references for the quality control of Ophiopogon japonicus in Shengmaiyin.
作者
黄赛燕
徐丹洋
姚奕然
王舒
钱洁
朱琳
刘欢欢
HUANG Saiyan;XU Danyang;YAO Yiran;WANG Shu;QIAN Jie;ZHU Lin;LIU Huanhuan(Nantong Food and Drug Control Center,Nantong 226014,Jiangsu Province,China)
出处
《药学前沿》
CAS
2024年第11期390-396,共7页
China Pharmacist
基金
江苏省药品专项抽检课题(苏药监办稽[2022]64号)。
关键词
生脉饮
麦冬
麦冬高异黄酮A
山麦冬皂苷B
短葶山麦冬皂苷C
超高效液相色谱-三重四级杆串联质谱法
Shengmaiyin
Ophiopogon japonicus
Methylophiopogonanone A
Liriopeside B
Liriope muscari baily saponin C
Ultra performance liquid chromatography tandem mass spectrometry
