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 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分别在浓度0.01~2μg·m L^(-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·m L^(-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98.89%、99.80%、100.61%、99.35%、99.51%,RSD%分别为0.84%、0.90%、1.19%、1.28%、0.86%。测定样品3批,5个成分的测定结果分别为:批号S154601:0.2605、0.2721、0.1848、0.1693、4.8203 mg·g^(-1);批号S154602:0.2440、0.2573、0.1709、0.1712、4.7639 mg·g^(-1);批号S154603:0.2679、0.2788、0.1900、0.1778、4.8725 mg·g^(-1)。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。
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.
出处
《中国药品标准》
CAS
2017年第6期455-460,共6页
Drug Standards of China
