肾康注射液中化学成分的UPLC-Q-TOF-MS分析

Analysis on chemical constituents in Shenkang Injection by UPLC-Q-TOF-MS

目的建立肾康注射液中的化学成分的超高效液相色谱仪联用四级杆串联飞行时间质谱仪(UPLC-Q-TOF-MS)分析方法。方法采用Waters Acquity HSS T3色谱柱(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液–乙腈,梯度洗脱;体积流量为0.4 m L/min;柱温为40.0℃;进样量为2.00μL。质谱检测采用正、负离子模式,电压分别为3.0、2.9k V;离子源温度120℃;脱溶剂气体温度450℃;脱溶剂气体体积流量900 L/h。结果鉴定出了肾康注射液中10个化合物,分别为没食子酸、芦荟大黄素-8-O-β-D-吡喃葡萄糖苷、丹参素、原儿茶醛、苯乙醛、芦荟大黄素、毛蕊异黄酮、云杉鞣酚-3'-O-葡萄糖苷、白藜芦醇-4'-O-葡萄糖苷、大黄素,并结合文献报道对其药材来源进行了归属。结论建立了一种简单、快速、高效的UPLC/Q-TOF-MS方法对肾康注射液中化学成分进行了鉴定,为阐明肾康注射液的物质基础提供了参考。

Objective To establish a method for the analysis on the chemical constituents in Shenkang Injection by UPLC-Q-TOF-MS. Methods The method was performed on Waters Acquity HSS T3 column （100 mm × 2.1 mm, 1.8 μm）, and the mobile phase consisted of 0.1% formic acid aqueous solution and acetonitrile with gradient elution program. The injection volume was 2.00 μL at the flow rate of 0.4 mL/min. The column temperature was 40.0 ℃. Both positive and negative modes were selected for qualitative analysis. The capillary voltages were set at 3.0 and 2.9 kV. The ion source temperature and atomization temperature were 120 and 450 ℃. The flow rate of nebulization gas was 900 L/h. Results Ten compounds in Shenkang Injection were identified as gallic acid, aloe-emodin-8-O-b-D-glucopyranoside, salvianic acid, protocatechualdehyde, phenylacetaldehyde, aloe-emodin, calycosin, piceatannol 3′-O-β-D-glucopyranoside, resveratrol-4＇-O-β-D-glucopyranoside, and emodin, and the source of medicinal materials was assigned according to the literature. Conclusion The established method for the determination of the chemical constituents in Shenkang Injection by UPLC-Q-TOF-MS is simple, rapid, and reliable, and provide a reference for clarifying the material basis of Shenkang Injection.