贾首时,王萌萌,王超众.HPLC-MS/MS法测定桑菊感冒片中5种成分的含量[J].中国药品标准,2017,18(6):455-460 |
HPLC-MS/MS法测定桑菊感冒片中5种成分的含量 |
Content Determinations of Five Components in Sangju Ganmao Tablets by HPLC-MS/MS |
投稿时间:2017-10-12 修订日期:2017-12-06 |
DOI: |
中文关键词: 高效液相色谱-串联质谱法 桑菊感冒片 芦丁 绿原酸 连翘苷 桔梗皂苷D 苦杏仁苷 含量 |
英文关键词: HPLC-MS/MS Sangju Ganmao Tablets rutin chlorogenic acid forsythin platycodin D amygdalin content |
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中文摘要: |
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Waters Atlantis C18色谱柱(2.1×150mm,5μm),以乙腈(A)-0.1%甲酸(B)为流动相,梯度洗脱(0~3min,20%A;3~15min,20%A→60%A;15~23min,60%A;23~24min,60%A→20%A;24~30min,20%A),流速0.2mL.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分别在浓度0.01~2 μg.mL-1的线性范围内线性关系良好(r>0.999),苦杏仁苷在浓度0.25~50μg.mL-1的线性范围内线性关系良好(r>0.999),平均回收率(n=6)分别为98.86%、99.80%、100.61%、99.35%、99.60%,RSD%分别为0.84%、0.90%、1.19%、1.28%、0.86%。结论:所建立的方法准确、可靠、重复性好,灵敏度高,为桑菊感冒片的全面质量控制提供科学依据。 |
英文摘要: |
Objective:To establish the method for determinations of rutin, chlorogenic acid, forsythin, platycodin D and amygdalin in Sangju Ganmao Tablets by HPLC-MS/MS. Methods:The determination was carried out with Waters Atlantis C18 column (2.1×150mm,5μm).The mobile phase consisted of acetonitrile(A)-0.1% formic acid solution(B) with gradient elution(0~3min,20%A;3~15min,20%A→60%A;15~23min,60%A;23~24min,60%A→20%A;24~30min,20%A) at a flow rate of 0.2 mL.min-1 at 35℃.The analytes were detected by tandem mass spectrometry with the electrospray ionization(ESI) source combined with multiple reaction monitoring(MRM) mode. Results:Rutin, chlorogenic acid, forsythin and platycodin D showed a good linearity in the range of 0.01~2μg.mL-1(r>0.999).The amygdalin showed a good linearity in the range of 0.25~50μg.mL-1(r>0.999). The average recoveries (n=6) were 98.86%,99.80%,100.61%,99.35%,99.60% with the RSD% were 0.84%、0.90%,1.19%,1.28%,0.86%.Conclusion:This method is reliable, accurate, which offers advantages of highy sensitivity and precision. It can be used for the overall assessment of the quality of Sangju Ganmao Tablets. |
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