摘要
目的:建立高效液相色谱-串联质谱法同时测定桑菊感冒片中芦丁、绿原酸、连翘苷、桔梗皂苷D和苦杏仁苷的含量。方法:采用Atlantis C_(18)色谱柱(2.1 mm×150 mm,5μm),以乙腈(A)-0.1%甲酸(B)为流动相,梯度洗脱(0~3 min,20%A;3~15 min,20%A→60%A;15~23 min,60%A;23~24 min,60%A→20%A;24~30 min,20%A),流速0.2 m L·min^(-1),柱温35℃,采用电喷雾离子源(ESI),以多反应监测(MRM)方式进行正离子扫描。结果:芦丁、绿原酸、连翘苷和桔梗苷D质量浓度均在0.01~2μg·m L^(-1)的范围内线性关系良好(r>0.999),苦杏仁苷质量浓度在0.25~50μg·m L^(-1)的范围内线性关系良好(r>0.999),平均回收率(n=6)分别为98.9%、99.8%、100.6%、99.4%、99.6%,RSD分别为0.84%、0.90%、1.2%、1.3%、0.86%;3批样品中芦丁、绿原酸、连翘苷、桔梗皂苷D和苦杏仁苷含量范围分别为244.0~267.9、257.3~278.8、170.9~190.0、169.3~177.8、4763.9~4872.5μg·g^(-1)。结论:所建立的方法为桑菊感冒片的全面质量控制提供科学依据。
Objective：To establish a method for the determination of rutin,chlorogenic acid,forsythin,platycodin D and amygdalin in Sangju Ganmao tablets by HPLC-MS/MS.Methods：The determination was carried out on an Atlantis C_（18） column（2.1 mm×150 mm,5μm）at 35℃.The mobile phase consisted of acetonitrile（A）-0.1%formic acid solution（B）with gradient elution（0-3 min,20%A;3-15 min,20%A→60%A;15-23 min,60%A;23-24 min,60%A→20%A;24-30 min,20%A）at a flow rate of 0.2 m L·min^（-1）.The analytes were detected by tandem mass spectrometry with the electrospray ionization（ESI）source combined with multiple reaction monitoring（MRM）modes.Results：Rutin,chlorogenic acid,forsythin and platycodin D showed good linearities in the range of 0.01-2μg·m L^（-1）（r0.999）.Amygdalin showed a good linearity in the range of 0.25-50μg·m L^（-1）（r0.999）.The average recoveries（n=6）were 98.9%,99.8%,100.6%,99.4%and 99.6%with RSDs of 0.84%,0.90%,1.2%,1.3%and 0.86%.The contents of rutin,chlorogenic acid,forsythin,platycodon D and amygdalin in 3 batches of samples were 244.0-267.9μg·g^（-1）,257.3-278.8μg·g^（-1）,170.9-190.0μg·g^（-1）,169.3-177.8μg·g^（-1） and 4 763.9-4 872.5μg·g^（-1）,respectively.Conclusion：This method can be used for the overall assessment of the quality of Sangju Ganmao tablets.
作者
崔爱湜
王萌萌
贾首时
王超众
李想
任雅慧
陈爽
CUI Ai-shi;WANG Meng-meng;JIA Shou-shi;WANG Chao-zhong;LI Xiang;REN Ya-hui;CHEN Shuang(Department of Pharmacy,The Third Affiliated Hospital of Qiqihar Medical University,Qiqihar 161002,China;Combination of Chinese Medicine and Western Medicine of the First Hospital of Qiqihar City,Qiqihar 161005,China;Qiqihar Institute for Food and Drug Control,Qiqihar 161005,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第7期1254-1261,共8页
Chinese Journal of Pharmaceutical Analysis
