参麦注射液超高效液相指纹图谱的建立及特征成分分析

目的: 采用超高效液相色谱(UPLC)建立参麦注射液指纹图谱,为直观、简便、全面地评价参麦注射液的质量提供依据. 方法: 采用UPLC建立参麦注射液的指纹图谱快速检测方法,并利用离子阱质谱联用技术对其特征性成分进行分析.色谱条件:实验采用Waters Acquity Uplc Hss T3色谱柱(100 mm×2.1 mm,1.8 μm),流动相为乙腈-水,梯度洗脱,流速0.4 mL·min^-1,检测波长203 nm.质谱检测条件:毛细管电压3.5 kV,雾化器压力206.9 Pa,离子源温度350 ℃,干燥气流12 L·min^-1,负离子模式扫描,扫描范围100~1300 m/z. 结果: 建立了全国3个厂家19批参麦注射液UPLC指纹图谱,利用多级质谱信息,结合对照品和文献对12个共有峰进行指认.19批参麦注射液除2批外相似度均高于0.85.聚类分析结果显示不同厂家的参麦注射液各自聚为一类. 结论: UPLC法测定参麦注射液指纹图谱,不仅可快速观察其生产工艺,并可为区分不同厂家的参麦注射液提供依据.

Objective: To establish a UPLC-PDA fingerprint of Shenmai injection for providing reference for visual,easy and overall control of the quality of Shenmai injection. Methods: In this research,UPLC fingerprints were established for quick inspection of Shenmai injections whose characteristic components were analyzed using Iron-Trap-MSⁿ. In the lab tests conducted for this research,the chromatographic separation was performed on a Waters Acquity Uplc Hss T3(100 mm×2.1 mm,1.8 μm)column. A gradient elution of water-acetonitrile as the mobile phase was used at a flow rate of 0.4 mL·min^-1. The detection wavelength was set at 203 nm. The condition of Iron-Trap-MSⁿ was set as follows:the capillary voltage at 3.5 kV,the nebulizer pressure at 206.9 Pa,the dry gas flow rate and the temperature at 12 L·min^-1 and 350 ℃,respectively. MSⁿ data was performed in negative mode. The mass range was set from 100 m/z to 1300 m/z. Results: Based on the results of lab tests,similarity comparison and cluster analysis were conducted for the fingerprints of 19 batches of Shenmai injection from three companies. Using MSⁿ information,together with the reference standards and literatures,12 common peaks were identified. Among the 19 batches of samples,17 of them had similarity degrees over 0.85. According to the cluster analysis,it was found that Shenmai injections collected from the same company clustered into the same category,therefore,Shenmain injections from different companies can be easily separated. Conclusion: The comparison and cluster analysis showed that the method presented in this paper can be used to perform fast and accurate assessment of the quality of Shenmai injection. It can also be used for quick and accurate distinction of Shenmain injections from different companies. This method can not only fast observe the production process of Shenmai injection,but also can provide the basis for quality evaluation of the injection.