基于UPLC-Q-TOF-MS技术对黄连须生物碱类成分及其裂解规律的分析

Analysis of Alkaloids and Their Fragmentation Behavior of Coptis Rootlet by UPLC-Q-TOF-MS

关键词:  黄连须  超高效液相色谱-飞行时间质谱联用技术  生物碱  裂解规律

Key words:  Coptis rootlet  UPLC-Q-TOF-MS  alkaloids  fragmentation behavior

摘要:

目的 应用超高效液相色谱-飞行时间质谱联用技术（ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry，UPLC-Q-TOF-MS）分析黄连须中生物碱类成分，并对其中主要类型生物碱的裂解规律进行解析。方法 采用Waters Acquity UPLC BEH C₁₈色谱柱，以0.1%甲酸水（A）-0.1%甲酸乙腈（B）为流动相，梯度洗脱，质谱采用电喷雾离子源，正负离子模式下采集数据，在Peakview 2.0/masterview 1.0软件中依据自建的黄连化学成分数据库筛查化合物，通过精确质量数及比对Natural Products HR-MS/MS Spectral Library 1.0 software所含的1 000余种中草药对照品二级谱图进行裂解规律分析。结果 鉴定并推断出黄连须中19个生物碱类成分，并对其中原小檗碱型、氧化小檗碱型及普罗托品型生物碱的裂解规律进行了分析。结论 该法为黄连须成分研究提供了依据，证明了黄连须的利用价值，并对其进一步开发利用奠定了基础。

Abstract:

OBJECTIVE To analysis alkaloids and their fragmentation behavior of Coptis rootlet by ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS). METHODS The separation was performed on the chromatographic column of Waters Acquity UPLC BEH C₁₈ by gradient elution with 0.1% formic acid water(A) and 0.1% formic acid acetonitrile(B). An electrospray ion source was used for mass spectrometry to collect data in both positive and negtive ion mode. Screening compounds in the Peakview 2.0/masterview 1.0 software based on the self-built Coptis chemistry database. The secondary spectra of more than 1 000 kinds of Chinese herbal medicine reference substances contained in Natural Products HR-MS/MS Spectral Library 1.0 software were analyzed by accurate mass number and comparison. RESULTS Nineteen alkaloids in Coptis rootlet were identified and inferred, and the fragmentation behavior of protoberberine, oxidized berberine and protopine alkaloids were analyzed. CONCLUSION This method provides a basis for the study of the constituents of Coptis rootlet, which proves the utilization of Coptis rootlet and lays a foundation for its further development and utilization.