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目的:建立油菜蜂花粉的HPLC指纹图谱,为其质量评价提供参考。方法:采用RP-HPLC法,色谱条件为Sinochrom ODS-AP(250 mm×4.6 mm,5μm)色谱柱;流动相为0.2%(V/V)磷酸水溶液(A相)和乙腈(B相)梯度洗脱,流速1.0 mL/min;检测波长260 nm;柱温30℃。在上述条件下,通过对11批不同产地的油菜蜂花粉样品色谱分析,建立其指纹图谱。应用中药色谱指纹图谱相似度评价系统(国家药典委员会2004A)进行相似度评价,并运用聚类分析(HCA)对指纹图谱进行模式识别。结果:共筛选出22个共有峰,经相似度评价,均大于0.90;方法学考察中共有峰相对保留时间和相对峰面积RSD分别小于1.0%和4.0%;不同产地油菜蜂花粉HPLC指纹图谱具有一定的差异;经聚类分析(HCA)模式识别,11批样品被分为2类。结论:建立的指纹图谱可对其质量评价及控制提供依据。
Objective: To establish HPLC fingerprinting of rape bee pollen and provide references for its quality evaluation. Methods: The chromatographic conditions were RP-HPLC on a Sinochrom ODS-AP column (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of a 0.2% (V / V) phosphoric acid aqueous solution Elution, flow rate 1.0 mL / min; detection wavelength 260 nm; column temperature 30 ℃. Under the above conditions, the fingerprints of eleven batches of rape bee pollen samples from different regions were established. Similarity evaluation was performed by using the similarity evaluation system of chromatographic fingerprints of Chinese medicine (State Pharmacopoeia Commission 2004A), and the fingerprints were identified by cluster analysis (HCA). Results: A total of 22 common peaks were screened, and the similarity was estimated to be greater than 0.90. The relative retention time (RSD) and relative peak area (RSD) of common peaks were less than 1.0% and 4.0%, respectively. HPLC fingerprinting of bee pollen from different regions had A certain difference. According to cluster analysis (HCA) pattern recognition, 11 batches of samples were divided into two categories. Conclusion: The established fingerprint can provide a basis for its quality evaluation and control.