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[大株红景天胶囊的HPLC-DAD-QTOF-MS指纹图谱]

[Fingerprint of Dazhu Hongjingtian capsule by HPLC-DAD-QTOF-MS].

作者信息

Liu Guang-da, Huang Wen-Zhe, Ma Shi-Ping, Wang Zhen-Zhong

机构信息

Jiangsu Kanion Pharmaceutical Co., Ltd., Lianyungang 222001, China.

China Pharmaceutical University, Nanjing 210009, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2016 Aug;41(16):3022-3026. doi: 10.4268/cjcmm20161613.

Abstract

A method was established to analyze the fingerprint of Dazhu Hongjingtian capsule by HPLC-DAD.The separation was performed on Agilent Eclipse Plus-C₁₈(4.6 mm×250 mm, 5 μm) with methanol-0.1% formic acid solution as the mobile phase for gradient elution at a flow rate of 1.0 mL•min⁻¹; the detection wavelength was set at 276 nm and column temperature was set at 35 ℃. A total of 10 batches of samples were detected by the above method, and based on their fingerprint by using Similarity Evaluation System for Chromatographic Fingerprint of TCM (2004A), 21 common chromatographic peaks were determined and after the individual common peak whose peak area was greater than 50% of the total peak area was deducted, the similarity results of these samples were analyzed and compared. The results showed that the similarity of 10 batches of samples was all higher than 0.940. HPLC/Q-TOF-MS was used to identify the common chromatographic peaks in the fingerprint and determine the molecular formulas of twenty-one common chromatographic peaks. The structures of 11 fingerprint peaks were tentatively identified based on the control products and mass spectrometry information. This was the first time to establish fingerprint by using HPLC method and identify fingerprint peaks by using HPLC/Q-TOF-MS. This method has good precision, stability and repeatability, and could provide basis for quality evaluation of Dazhu Hongjingtian capsule.

摘要

建立了一种采用高效液相色谱-二极管阵列检测器(HPLC-DAD)分析大株红景天胶囊指纹图谱的方法。采用安捷伦Eclipse Plus-C₁₈色谱柱(4.6 mm×250 mm,5 μm),以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱,流速为1.0 mL•min⁻¹;检测波长设定为276 nm,柱温设定为35℃。采用上述方法对10批样品进行检测,依据《中药色谱指纹图谱相似度评价系统》(2004A版)对其指纹图谱进行分析,确定了21个共有色谱峰,扣除峰面积大于总峰面积50%的单峰后,对这些样品的相似度结果进行分析比较。结果表明,10批样品的相似度均高于0.940。采用HPLC/Q-TOF-MS对指纹图谱中的共有色谱峰进行鉴定,并确定了21个共有色谱峰的分子式。根据对照品及质谱信息对11个指纹峰的结构进行了初步鉴定。首次采用HPLC法建立指纹图谱,并采用HPLC/Q-TOF-MS对指纹峰进行鉴定。该方法精密度、稳定性及重复性良好,可为大株红景天胶囊的质量评价提供依据。

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