Key Laboratory of Chinese MateriaMedica, Heilongjiang University of Chinese Medicine, Ministry of Education, Harbin 150040, China
Molecules. 2017 Nov 24;22(12):2057. doi: 10.3390/molecules22122057.
The Shuang-Huang-Lian (SHL) oral liquid is a combined herbal prescription used in the treatment of acute upper respiratory tract infection, acute bronchitis and pneumonia. Multiple constituents are considered to be responsible for the therapeutic effects of SHL. However, the quantitation of the multi-components from multiple classes is still unsatisfactory because of the high complexity of constituents in SHL. In this study, an accurate, rapid, and specific UPLC-MS/MS method was established for simultaneous quantification of 18 compounds from multiple classes in SHL oral liquid formulations. Chromatographic separation was performed on a HSS T3 (1.8 μm, 2.1 mm × 100 mm) column, using a gradient mobile phase system of 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.2 mL·min; the run time was 23 min. The MS was operated in negative electrospray ionization (ESI) for analysis of 18 compounds using multiple reaction monitoring (MRM) mode. UPLC-ESI-MRM-MS/MS method showed good linear relationships (² > 0.999), repeatability (RSD < 3%), precisions (RSD < 3%) and recovery (84.03-101.62%). The validated method was successfully used to determine multiple classes of hydrophilic and lipophilic components in the SHL oral liquids. Finally, principal component analysis (PCA) was used to classify and differentiate SHL oral liquid samples attributed to different manufacturers of China. The proposed UPLC-ESI-MRM-MS/MS coupled with PCA has been elucidated to be a simple and reliable method for quality evaluation of SHL oral liquids.
双黄连口服液是一种复方草药制剂，用于治疗急性上呼吸道感染、急性支气管炎和肺炎。多种成分被认为是双黄连口服液发挥治疗作用的原因。然而，由于双黄连口服液成分的高度复杂性，对多类成分的定量分析仍不尽如人意。本研究建立了一种准确、快速、特异的 UPLC-MS/MS 法，用于同时定量分析双黄连口服液制剂中多类 18 种化合物。色谱分离在 HSS T3（1.8 μm，2.1 mm×100 mm）柱上进行，采用 0.1%甲酸乙腈和 0.1%甲酸水为流动相，梯度洗脱，流速为 0.2 mL·min；运行时间为 23 min。MS 采用负离子电喷雾电离（ESI）模式，以多反应监测（MRM）模式分析 18 种化合物。UPLC-ESI-MRM-MS/MS 法显示出良好的线性关系（²＞0.999）、重复性（RSD＜3%）、精密度（RSD＜3%）和回收率（84.03-101.62%）。该验证方法成功地用于测定双黄连口服液中的多类亲水性和疏水性成分。最后，采用主成分分析（PCA）对来源于中国不同厂家的双黄连口服液样品进行分类和区分。该研究表明，UPLC-ESI-MRM-MS/MS 与 PCA 相结合，可用于双黄连口服液的质量评价。
