LC-MS快速分析紫苏水煎液中的主要化学成分

目的: 采用液相色谱,结合四极杆飞行时间串联质谱(QTOF/MS)和离子阱质谱(IT/MS)2种质谱检测器,分析鉴定中药紫苏水煎液中的主要化学成分。方法: 色谱柱为ZorbaxSB-C₁₈RRHD柱(4.6 mm×50 mm,1.8 μm),以0.05%甲酸水溶液- 乙腈为流动相,梯度洗脱,流速为0.5 mL·min^-1,柱温30℃,进样体积10 μL;采用QTOF获取化合物的分子式,并用数据依赖扫描辨别质核比接近的离子碎片;结合IT/MS的多级质谱分析推断可能的结构并验证鉴定结果。结果: 通过联合使用2种不同原理的质谱仪并参照数据库和文献资料从紫苏水煎液中鉴定了27个化合物,包括9个黄酮及其苷类成分,10个有机酸类成分,5个氨基酸、2个缩氨酸和1个核苷,其中4个成分经由对照品比对确证。结论: 该方法通过联合使用QTOF/MS和IT/MS,为化合物的快速解析提供了更多数据,提高了分析的速度和准确性,为中药复杂组分的分析提供了一种可行的方法。

Objective: To identify the chemical constituens in the decoction of Perilla frutescens by liquid chromatography-ion trap and quadrupole time-of-flight mass spectrometry. Methods: A Zorbax SB-C₁₈RRHD (4.6 mm×50 mm, 1.8 μm) column was used for chromatographic separation with column temperature maintained at 30℃; 0.05% formic acid-water and acetonitrile was employed as mobile phase in a gradient elution program; the flow rate was set at 0.5 mL·min^-1, and the injection volume was 10 μL; QTOF was used to generate the molecular formula and identify fragment ions with identical nominal masses, while IT/MS was used to perform multistage MS analysis. Results: A total of 27 compounds was identified from the decoction of Perilla frutescens, including nine flavonoids, ten organic acids, five amino acids, two peptides and one nucleoside, four of which were unambiguously identified via comparison with chemical standards. Conclusion: The combination of QTOF/MS and IT/MS has the complementary advantages and more MS data for characterization of chemical constituents in traditional Chinese medicine.The established methodology provides a feasible approach for analysis of complex herbal medicines.