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[超快速液相色谱-四极杆-飞行时间串联质谱法快速分析芪葛颗粒中的化学成分]

[Rapid analysis on chemical constituents in Qige Keli by RRLC-Q-TOF-MS/MS].

作者信息

Yin Hui-Min, 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(21):4240-4247. doi: 10.19540/j.cnki.cjcmm.20180807.003.

Abstract

The qualitative analysis method of RRLC-Q-TOF-MS/MS was established for determine the chemical constituents in Qige Keli. Kramosil C₁₈ column (4.6 mm×150 mm, 3.5 μm) was used at the temperature of 30 °C. The mobile phase was 0.2% formic acid and acetonitrile by gradient elution, with a flow rate at 1.0 mL·min⁻¹, and the injection volume was 10 μL. The high-resolution quadrupole time-flight mass spectrometry was used as detector with electrospray ion source in both positive and negative models. On the basis of medicinal materials, reference materials, literature reports, and mass spectrometry data, the chemical composition in the Qige Keli was identified. A total of 44 compounds were identified, including 3 flavonoids, 21 flavonoid glycosides, 8 organic acids, 6 lactones, and 3 saponins. The results laid the foundation for the quality control of Qige Keli and the further research on pharmacodynamic materials.

摘要

建立了快速反向液相色谱-四极杆-飞行时间串联质谱(RRLC-Q-TOF-MS/MS)定性分析方法,用于测定芪葛颗粒中的化学成分。采用Kramosil C₁₈色谱柱(4.6 mm×150 mm,3.5 μm),柱温30℃。流动相为0.2%甲酸溶液和乙腈,梯度洗脱,流速为1.0 mL·min⁻¹,进样量为10 μL。采用高分辨四极杆飞行时间质谱作为检测器,电喷雾离子源,正、负离子模式采集数据。依据药材、对照品、文献报道及质谱数据,对芪葛颗粒中的化学成分进行了鉴定。共鉴定出44个化合物,包括3个黄酮类、21个黄酮苷类、8个有机酸类、6个内酯类和3个皂苷类。该结果为芪葛颗粒的质量控制及药效物质基础的进一步研究奠定了基础。

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