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

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)

机构地区：[1]南通市食品药品监督检验中心,江苏南通226014

出　　处：《药学前沿》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)。

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.

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 

分 类 号：R286.0[医药卫生—中药学]