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HPLC-MS/MS法测定桑菊感冒丸中3种成分的含量
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| 篇名： | HPLC-MS/MS法测定桑菊感冒丸中3种成分的含量 |
| TITLE： | |
| 摘要： | 目的：建立同时测定桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的方法。方法：采用高效液相色谱-串联质谱法。色谱柱为Waters Atlantis C18，流动相为乙腈-0.1％甲酸溶液（梯度洗脱），流速为0.2 mL/min，柱温为35 ℃，进样量为10 μL。离子源为电喷雾离子源，采用多反应监测扫描模式和正离子检测模式，干燥气和雾化气均为高纯氮气，干燥气温度为270 ℃，干燥气流量为25 L/min，鞘气流量为10 L/min，毛细管电压为4 500 V，喷嘴电压为2 000 V，扫描时间为0.1 s。结果：芦丁、连翘苷和桔梗皂苷D检测质量浓度线性范围分别为0.010 82～2.164 μg/mL（r＝0.999 7）、0.010 18～2.036 μg/mL（r＝0.999 4）、0.010 27～2.054 μg/mL（r＝0.999 7）；定量限分别为1.250、0.260、2.720 ng/mL，检测限分别为0.380、0.078、0.820 ng/mL；精密度、稳定性、重复性试验的RSD＜3.0％；加样回收率分别为97.88％～99.88％（RSD＝0.72％，n＝6）、98.48％～103.13％（RSD＝1.91％，n＝6）、98.79％～101.41％（RSD＝1.05％，n＝6）。结论：该方法操作简便，精密度、稳定性、重复性好，可用于桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的同时测定。 |
| ABSTRACT： | OBJECTIVE： To establish the method for simultaneous determinations of rutin， forsythin and platycodin D in Sangju ganmao pills. METHODS： HPLC-MS method was adopted. The determination was performed on Waters Atlantis C18 column with mobile phase consisted of acetonitrile-0.1％ formic acid （gradient elution） at the flow rate of 0.2 mL/min. The column temperature was set 35 ℃， and sample size was 10 μL. The ionization mode was electrospray ion， and the reaction mode was multi-reaction monitoring. By positive ion detection mode， the drying gas and nebuliser gas were all high purity nitrogen. The drying gas temperature was 270 ℃.The drying gas flow rate was 25 L/min. The sheath gas flow rate was 10 L/min. The capillary voltage was 4 500 V. The nozzle voltage was 2 000 V and the scanning time was 0.1 s. RESULTS： The linear range of rutin， forsythin and platycodin D were 0.010 82-2.164 μg/mL （r＝0.999 7）， 0.010 18-2.036 μg/mL （r＝0.999 4），0.010 27-2.054 μg/mL （r＝0.999 7）， respectively. The limits of quantification were 1.250，0.260，2.720 ng/mL， and the limits of detection were 0.380，0.078， 0.820 ng/mL. RSDs of precision， stability and reproducibility tests were all no more than 3.0％. The recoveries were 97.88％-99.88％ （RSD＝0.72％，n＝6），98.48％-103.13％（RSD＝1.91％，n＝6）， 98.79％-101.41％（RSD＝1.05％，n＝6）. CONCLUSIONS： This method is simple， precise， stable and reproducible， and can be used for simultaneous determination of rutin， forsythin and platycodin D in Sangju ganmao pills. |
| 期刊： | 2017年第28卷第36期 |
| 作者： | 刘世军，孙克明，刘宪勇，张敏，谷雨，王岩，毕文超，魏玮 |
| AUTHORS： | LIU Shijun，SUN Keming，LIU Xianyong，ZHANG Min，GU Yu，WANG Yan，BI Wenchao，WEI Wei |
| 关键字： | 高效液相色谱-串联质谱法；桑菊感冒丸；芦丁；连翘苷；桔梗皂苷D；含量 |
| KEYWORDS： | HPLC-MS/MS； Sangju ganmao pills； Rutin； Forsythin； Platycodin D； Content |
| 阅读数： | 344 次 |
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