金丝苦楝的化学成分鉴定及不同产地金丝苦楝的6种黄酮类成分含量测定

    Identification of Chemical Constituents of Cardiospermum Halicacabum L. and Content Determination of Six Flavonoid Components of Cardiospermum Halicacabum L. from Different Regions

    • 摘要:
      目的  基于超高效液相色谱-串联四极杆飞行时间质谱(UPLC-Q/TOF-MS/MS) 分析金丝苦楝药材的化学成分,并基于HPLC建立同时测定不同产地金丝苦楝的6种黄酮类成分含量的方法。
      方法 UPLC-Q/TOF-MS/MS采用Cortecs UPLC C18色谱柱(2.1 mm×100 mm,1.6 μm),流动相甲醇(A)-0.1%甲酸水(B)梯度洗脱,流速0.2 mL·min−1,柱温35 ℃,进样量2 μL。MS条件:电喷雾正、负离子模式采集数据,质谱扫描范围m/z 50~1000。HPLC采用Shim-pack GIST C18色谱柱(4.6 mm×250 mm,5 μm),流动相为甲醇(A)-0.1%甲酸水(B),梯度洗脱,流速1 mL·min−1,柱温35 ℃,检测波长350 nm,进样量10 μL。使用 SIMCA-P 14.1进行主成分分析,筛选得到差异性(VIP>1)的成分。
      结果 基于 UPLC-Q/TOF-MS/MS 技术在正、负离子模式下鉴定出33个化合物;基于HPLC测定不同产地金丝苦楝的6种黄酮类成分,进行主成分分析,结果显示福建、广东、广西3个产地的金丝苦楝各自聚为一类,不同批次金丝苦楝的主要差异性成分为木犀草素-7-O-葡萄糖醛酸苷、异槲皮苷、芹菜素-7-O-葡萄糖醛酸苷,不同产地的样品存在较大差异,同时通过研究发现广西产的金丝苦楝样品组间差异小,质量较稳定。
      结论 基于UPLC-Q-TOF-MS/MS技术,可实现对金丝苦楝药材化学成分的快速鉴定,建立的HPLC测定金丝苦楝中6种黄酮类成分的含量方法稳定、可靠,可为其质量控制提供参考。

       

      Abstract:
      OBJECTIVE  To analyze the chemical components of Cardiospermum halicacabum L. using UPLC-Q/TOF-MS/MS and establish a method for simultaneous determination of six flavonoid components in Cardiospermum halicacabum L. from different regions using HPLC.
      METHODS  UPLC-Q/TOF-MS/MS was performonced on Cortec UPLC C18 column(2.1 mm×100 mm, 1.6 μm) with mobile phase of methanol(A)-0.1% formic acid water(B) in gradient elution, with the flow rate of 0.2 mL·min−1, the column temperature of 35 ℃, injection volume of 2 μL; electrospray ionization(ESI) source was used to acquire mass spectrometry data in positive and negative ion modes with the scanning range of m/z 50–1 000. HPLC was performed on Shim-pack GIST C18(4.6 mm×250 mm, 5 μm) with mobile phase consisting of methanol(A) -0.1% formic acid water(B) in gradient elution, with the flow rate of 1 mL·min−1, column temperature of 35 ℃, detection wavelength of 350 nm, and injection volume of 10 μL. Principal component analysis(PCA) was conducted using SIMCA-P 14.1, and the components with significant differences(VIP>1) were screened.
      RESULTS  Utilizing the UPLC-Q/TOF-MS/MS technique, a total of 33 compounds were identified in both positive and negative ion modes. Based on the HPLC method, six flavonoid components were identified and PCA was conducted. The results of PCA showed that the Cardiospermum halicacabum L. from Fujian, Guangdong and Guangxi were grouped into one class respectively. The primary differential components in different batches of Cardiospermum halicacabum L. were luteolin-7-O-glucuronide, isoquercetin, and apigenin-7-O-glucuronide. Significant variations were observed among samples from different regions, while there was little difference between the samples of Cardiospermum halicacabum L. from Guangxi, and the quality was stable.
      CONCLUSION Based on the UPLC-Q-TOF-MS/MS technique, rapid identification of chemical components of Cardiospermum halicacabum L. is realized. The established HPLC method for the determination of 6 flavonoids in Cardiospermum halicacabum L. is stable and reliable, which can provide reference for quality control.

       

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