续断及其配方颗粒的UPLC指纹图谱研究

UPLC Fingerprinting Study of Dipsacus asper Wall. and Its Formulated Granules

摘要: 目的：建立续断药材及配方颗粒的UPLC指纹图谱，为续断配方颗粒质量控制提供有效方法。方法：采用UPLC同时测定10批续断药材和10批配方颗粒，制定指纹图谱。色谱柱为Agilent ZORBAX Eclipse Plus C₁₈ (2.1 mm × 100 mm, 1.8 μm)；流速0.2 mL·min⁻¹；检测波长212 nm；柱温30℃；进样量1 μL；流动相：0.1%磷酸水(A)-乙腈(C)二元梯度洗脱。结果：10批续断药材有25个共有色谱峰，10批续断配方颗粒有32个共有色谱峰，10批续断药材与10批配方颗粒确定25个共有峰，各峰之间分离度较高。10批续断药材和10批配方颗粒的相似度均大于0.8，10批配方颗粒的相似度大于0.9。结论：建立的续断药材和配方颗粒指纹图谱稳定可靠，药材与配方颗粒的色谱峰个数有较大的差异，说明药材经提取、浓缩、制粒等制备工艺后，化学成分有所变化，存在差异。

Abstract: Objective: To establish the UPLC fingerprints of Dipsacus asper W. and formulated granules, and to provide an effective method for the quality control of the formulated granules of Dipsacus asper W. Methods: UPLC was used to simultaneously determine 10 batches of Dipsacus asper W. and 10 batches of the formulated granules of Dipsacus asper W. and to develop the fingerprint profiles. The chromatographic column was Agilent ZORBAX Eclipse plus C18 (2.1 mm × 100 mm, 1.8 μm); the flow rate was 0.2 mL∙min⁻¹; the detection wavelength was 212 nm; the column temperature was 30˚C; the injection volume was 1 μL; and the mobile phase was a binary gradient elution of 0.1% phosphoric acid in water (A)-acetonitrile (C). Result: There were 25 common chromatographic peaks in 10 batches of Dipsacus asper W., 32 common chromatographic peaks in 10 batches of Formula granules, and 25 common peaks were determined between 10 batches of Dipsacus asper W. and 10 batches of formula particles, with high separation between each peak. The similarity between 10 batches of Dipsacus asper W. and 10 batches of formula particles is greater than 0.8, and the similarity between 10 batches of formula particles is greater than 0.9. Conclusion: The fingerprints of Dipsacus asper W. and Formula granules were stable and reliable and the number of chromatographic peaks of the herbs and the formulated particles had a large difference, indicating that the chemical compositions of the herbs had changed and differed after the preparation process of extraction, concentration and granulation.