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[基于超高效液相色谱-四极杆飞行时间串联质谱法快速鉴定杏贝止咳颗粒中的化学成分]

[Rapid identification of chemical components in Xingbei Zhike Keli by UPLC-Q-TOF-MS/MS].

作者信息

Zhang Ning, Gao Xia, Zhou Yu, Geng Ting, Yang Biao, Wang Xue, Huang Wen-Zhe, Xiao Wei

机构信息

College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.

State Key Laboratory of New-tech for Chinese Medicine Pharmaceutical Process, Lianyungang 222001, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2018 Nov;43(22):4439-4449. doi: 10.19540/j.cnki.cjcmm.20180807.004.

Abstract

To analyze and identify the chemical components in Xingbei Zhike Keli by using ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS). The analysis was performed on Agilent Zorbax SB-C₁₈(4.6 mm×250 mm, 5 μm) column, with methanol-0.08% formic acid solution (including 0.1% ammonium formate) as the mobile phase for gradient elution. The flow rate was 1 mL·min⁻¹ and column temperature was 30 °C. The MS spectrum was acquired in both negative and positive ion modes by using electron spray ionization (ESI). These components were further analyzed based on accurate m/z, secondary fragmentation and other information combined with reference substance and literature data. As a result, 87 compounds were successfully identified and predicted, including alkaloids, flavonoids, coumarins and saponins, of which 23 compounds were verified by comparing with reference substances. These results provide reference for the quality control of Xingbei Zhike Keli, and lay the foundation for elucidating their effective components and mechanism of action.

摘要

采用超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS/MS)对杏贝止咳颗粒中的化学成分进行分析和鉴定。分析在安捷伦Zorbax SB-C₁₈(4.6 mm×250 mm,5 μm)色谱柱上进行,以甲醇-0.08%甲酸溶液(含0.1%甲酸铵)为流动相进行梯度洗脱。流速为1 mL·min⁻¹,柱温为30℃。采用电喷雾电离(ESI)在负离子和正离子模式下采集质谱图。结合对照品和文献数据,根据精确的m/z、二级碎片等信息对这些成分进行进一步分析。结果成功鉴定和预测了87种化合物,包括生物碱、黄酮类、香豆素类和皂苷类,其中23种化合物通过与对照品比较得到验证。这些结果为杏贝止咳颗粒的质量控制提供了参考,为阐明其有效成分和作用机制奠定了基础。

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