UPLC-MS/MS测定生脉饮中麦冬及其掺伪品的3种特征成分
Determination of three characteristic components of Ophiopogon japonicus and its adulterants in Shengmaiyin by UPLC-MS/MS
黄赛燕 1徐丹洋 1姚奕然 1王舒 1钱洁 1朱琳 1刘欢欢1
作者信息
- 1. 南通市食品药品监督检验中心(江苏南通 226014)
- 折叠
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,2.6 μm),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1 μL;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0.016 7～1.666 0、0.039 7～15.872 0、0.022 5～8.988 0 ng(r≥0.999 9),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.
Abstract
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,2.6 μm)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 1 μL.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 0.016 7-1.666 0,0.039 7-15.872 0 and 0.022 5～8.988 0 ng(r＞0.999 9),respectively.The average recovery rates of these three components were 85.16％,86.95％and 95.07％,respectively,with RSSDs 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.
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Key words
Shengmaiyin/Ophiopogon japonicus/Methylophiopogonanone A/Liriopeside B/Liriope muscari baily saponin C/Ultra performance liquid chromatography tandem mass spectrometry引用本文复制引用
出版年
2024
NETL
NSTL
万方数据