基于水溶性浸出物及HPLC指纹图谱评价不同贮存年限半夏的品质

研究不同贮存年限半夏药材的浸出物,建立浸出物的HPLC特征指纹图谱,为半夏药材品质评控提供参考。浸出物测定方法采用药典法;HPLC指纹图谱的色谱条件:采用C_(18)色谱柱(150 mm×4.6 mm,5μm),以水–甲醇为流动相,梯度洗脱,流量为0.8 m L/min,检测波长为260 nm,柱温为25℃,进样体积为50μL。采用相似度评价及聚类分析技术揭示14批样品的相似性及差异性。14批半夏浸出物有12批合格,2批不合格。建立14批半夏浸出物样品的高效液相指纹图谱,确定了3个共有峰,共有峰保留时间的相对标准偏差小于2%,峰面积的相对标准偏差差异较大。1~#~7~#半夏样品有12个共有峰,共有峰保留时间的相对标准偏差小于1.5%,峰面积的相对标准偏差差异较大。各批次药材化学成分组成及含量均存在一定差异。以半夏浸出物数据与其高效液相色谱指纹图谱数据为基础,将指纹图谱相似度评价与聚类分析结合起来,用浸出物含量及评价软件测评结果对半夏品质进行综合评估,可以更精确地对半夏药材进行质量控制。

Quality Evaluation of Pinellia Ternata of Different Reserve Time Based on Water-Soluble Extract and HPLC Fingerprint

HPLC fingerprint of Pinellia Ternata was established which were derived from different harvest time and provided reliable method and scientific basis for their quality control. The contents of water–soluble extract was determined by Chinese Pharmacopoeia. The HPLC fingerprint chromatographic separation was achieved on a C18 column (150 mm×4.6 mm, 5μm), water and methanol solution was used as mobile phase in gradient elution program with the flow rate of 0.8 mL/min, the column temperature of 25℃, the injection volumeof 50μL and the detection wavelength of 260 nm. The similarity evaluation and clustering analysis were used to reveal similarities and differences in 14 batches of samples. The extract of 12 batches in 14 batches Pinelliae Rhizoma were qualified and 2 batches failed. The HPLC fingerprint of 14 batches of Pinelliae Rhizoma extract were set up and 3 common peaks were obtained, the RSD of the relative retention time of the common peaks was below 2%, the RSD of the relative peak area was difference. 1#–7# samples had 12 common peaks, the RSD of the relative retention time of the common peaks was below 1.5%, the RSD of the relative peak area was difference. 14 batches of medicinal in chemical composition and content were difference. Based on water-soluble extract data and HPLC fingerprint data and combined the fingerprint similarity evaluation system and cluster analysis, this comprehensive evaluation can be more precise for the Pinelliae Rhizoma quality control.