基于UPLC-Q-TOF-MS技术的银星养脑方化学成分分析

Identification of chemical constituents in Yinxing Yangnao Prescription by UPLC-Q-TOF-MS

目的:对银星养脑方的化学成分进行快速分析与鉴定,阐明其所含部分化合物可能的裂解途径。方法:采用超高效液相色谱串联四极杆飞行时间质谱联用技术(UPLC-Q-TOF-MS)对银星养脑方的化学成分进行快速分析与鉴定,色谱柱为ACQUITY UPLC BEH C18 column (2.1 mm×100 mm,1.7μm),以0.1%甲酸水-乙腈为流动相,梯度洗脱,体积流量0.4mL·min–1。采用正、负离子模式扫描,扫描范围m/z 50~1 500。根据精确质荷比和二级碎片离子信息,结合对照品和文献数据鉴定银星养脑方中的化学成分。结果:共鉴定出86个化学成分,包括苯丙素类、黄酮类、萜类、生物碱类、糖苷类、苯酞类、酚类、寡糖酯类、甾体类等,并对黄酮类、苯丙素类和萜类等成分进行裂解途径分析。结论:该方法快速准确,可作为银星养脑方化学成分快速分析与鉴别,并阐明了部分化学成分可能的裂解途径,为银星养脑方质量控制和物质基础研究提供理论依据。

OBJECTIVE To rapidly identify the chemical constituents of Yinxing Yangnao Prescription and clarify the possible cleavage pathway of some chemical constituents.METHODS Ultra performance liquid chromatography-quadrupole timeof-flight mass spectrometry(UPLC-Q-TOF-MS) was developed for rapid analysis and identification of chemical constituents of Yinxing Yangnao Prescription.The chromatographic column was ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm).Mobile phase was composed of 0.1% formic acid water-acetonitrile with gradient elution with a flow rate of 0.4 mL·min–1.Positive and negative ion modes were utilized for scanning with an range of m/z 50-1 500.According to the accurate mass-tocharge ratio and secondary fragment ion information,in conjunctions with reference substances and literature data,the chemical constituents in Yinxing Yangnao Prescription were identified.RESULTS A total of 86 chemical constituents were identified,including phenylpropanoids,flavonoids,terpenoids,alkaloids,glycosides,phthalides,phenols,oligosaccharide esters and steroids.The cleavage pathways of flavonoids,phenylpropanoids and terpenoids were analyzed.CONCLUSION The method is rapid and accurate so that it may be used as a rapid analysis and identification of chemical constituents of Yinxing Yangnao Prescription.Also the possible cleavage pathways of some chemical constituents are clarified.It provides theoretical rationales for quality controls and material basis researches of Yinxing Yangnao Prescription.