真元颗粒干浸膏HPLC-DAD指纹图谱和HPLC-MS/MS定性研究

Chromatographic Fingerprinting Study of Zhenyuan Granules Dry Extract by HPLC-DAD and HPLC-MS/MS

目的：应用HPLC-DAD建立真元颗粒干浸膏的指纹图谱分析方法,并进行药材归属研究;利用HPLCMS/MS法对色谱峰进行定性研究。方法：采用Agilent SB C18色谱柱（250 mm×4.6 mm,5μm）;流动相为0.1%甲酸乙腈溶液-0.1%甲酸溶液,梯度洗脱;流速1.2 m L/min（0~70 min）,0.8 m L/min（70~150 min）;柱温30℃;检测波长254 nm。结果：以甘草苷为参照峰,确定了40个共有峰,10批次真元颗粒干浸膏指纹图谱相似度良好（≥0.989）,且对27个色谱峰进行了成分定性分析。结论：该方法简便可靠,为全面有效控制真元颗粒质量提供了依据。

Objective： To establish a novel,accurate and valid fingerprint method of Zhenyuan granules dry extract by using HPLCDAD method,to study herbs belonging of fingerprint peaks and to identify some of the chromatographic peaks by HPLC-MS/MS analysis,for providing the basis for scientific evaluation of the quality. Methods： The sample solutions were analyzed by an Agilent SB C18（ 250 mm × 4. 6 mm,5 μm） column,and gradiently eluted with acetonitrile（ containing 0. 1% formic acid） and aqueous phase（ containing 0. 1% formic acid） as the mobile phase. The flow rates were 1. 2 m L/min（ 0 ~ 70 min） and 0. 8 m L/min（ 70 ~ 150 min）; the column temperature was 30 ℃; and the detection wavelength was 254 nm. Results： 40 peaks were selected as fingerprint peaks under the optimal chromatographic condition,and the similarity coefficients of 10 batches of Zhenyuan granules dry extract were all greater than0. 98. 27 peaks were tentatively identified with reference to literature data based on their mass spectrometry. Conclusion： The chromatographic fingerprint of Zhenyuan granules is proved to be a reliable method for comprehensive quality control and assessment.