龙血通络胶囊中化学成分的RRLC-Q-TOF MS分析

Characterization of constituents in Longxue Tongluo capsules by RRLC-Q-TOF MS

目的:采用快速液相色谱结合四极杆飞行时间串联质谱分析龙血通络胶囊中的主要化学成分。方法:采用Kromasil C18(4.6 mm×150 mm,3.5μm)色谱柱,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,进样体积5μL;质谱定性鉴别采用正负离子扫描模式,毛细管电压4 k V,雾化气压力275.8 k Pa,干燥气流速10 L·min-1,加热毛细管温度350℃,质量数扫描范围m/z 100~1 000,碰撞能量为15~30 V。结果:通过四极杆串联飞行时间质谱和碎片离子裂解分析,从龙血通络胶囊中鉴定出32个化学成分,包括29个黄酮类成分和3个二苯乙烯类成分,其中15个成分经由对照品比对确证。结论:所建立的RRLC-Q-TOF MS方法,可为鉴定龙血通络胶囊中化学成分提供一种快速、高效的方法,对其质量控制和药效物质基础研究具有重要意义。

Objective：To analyze and identify the chemical constituents of Longxue Tongluo capsules by rapid resolution liquid chromatography-quadrupole time-of-flight tandem mass spectrometry（RRLC-Q-TOF MS）.Methods：A Kromasil C18（4.6 mm×150 mm,3.5 μm）column was used for chromatographic separation withcolumn temperature maintained at 30 ℃.Acetonitrile and 0.01% formic acid were employed as mobile phase in a gradient elution program.The flow rate was set at 1.0 mL·min^（-1） and the injection volume was 5 μL.Quadrupole time-of-flight tandem mass spectrometry（Q-TOF MS）was applied to qualitative analysis in both positive and negative ion modes.The capillary voltage was 4 k V and the nebulizer gas pressure was 275.8 k Pa.The flow rate of the drying gas was 10 L·min-1 at a temperature of 350 ℃.The MS scan range was m/z1 000.The collision energy was 15-30 V.Results 100-：A total of 32 chemical constituents were identified in Longxue Tongluo capsules including 29 C flavonosiidosn and 3 stilbenoids,15 of which were unambiguously identified via comparison with chemical standards.onclu：A rapid and efficient RRLC-Q-TOF MS approach was established for studying the chemical constituents in Longxue Tongluo capsules.Furthermore,this study was significant to the quality control and the effective substances investigation of Longxue Tongluo capsules.