UPLC/Q-TOF MS法对注射用活血通络化学成分的初步分析

目的：采用液相色谱与四极杆飞行时间质谱（UPLC-QTOF/MS）联用技术，对活血通络粉针剂中的化学成分进行定性鉴别。方法：采用Themro（3 mm×100 mm，1.7μm）色谱柱，以甲醇-0.02%甲酸为流动相，梯度洗脱，体积流量为0.4 mL·min-1，柱温为30℃，进样量为3μL。检测质谱采用电喷雾离子源（ESI）的飞行时间质谱，正、负离子模式下采集数据，全扫描的质量扫描范围m/z 100～800。结果：结合UPLC-QTOF/MS提供的化合物准确相对分子质量及其二级质谱数据、对照品信息、相关文献数据对活血通络粉针化学成分进行鉴定并对化合物的药材来源进行了归属，共鉴定出18个化学成分。结论：UPLC-QTOF/MS法快速、准确、全面地鉴定活血通络粉针中的多种成分，为其质控和药效物质基础研究提供一定的参考。

Preliminary analysis of compounds in Huoxue Tongluo sterile powder by UPLC/QTOF MS

Objective: To analyze and identify the chemical components in Huoxue Tongluo sterile powder using ultra-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry (UPLC-QTOF/MS). Methods: A Themro column (3 mm ×100 mm, 1.7μm) was used for separation of the chemical components in Huoxue Tongluo sterile powder, with a mobile phase consisting of methanol (A) and water containing 0.02% formic acid (B) for gradient elution. The flow rate was 0.4 mL·min-1, the temperature of column was 30℃, with injection volume of 3μL. TOF/MS and electrospray ion (ESI) source were applied for the qualitative analysis under the positive and negative ion mode, and the full mass scan range was m/z 100-800. Results: The constituents from Huoxue Tongluo sterile powder were identified based on the relative molecule weight and secondary MS data from UPLC-QTOF/MS, reference substance information and related articles. All the peaks were assigned to the corresponding traditional Chinese medicinal materials with eighteen compounds identified. Conclusion: The method established is simple and rapid for elucidating the constituents of Huoxue Tongluo sterile powder and can be used for its quality control.