目的 建立复方仙灵骨葆胶囊(XLGB)的超高效液相色谱(UPLC)指纹图谱,结合化学计量学方法对多批次市售制剂进行质量评价。方法 采用ACQUITY UPLC BEH Shield RP18色谱柱 (2.1 mm×50 mm, 1.7 μm);以乙腈-水(各含体积分数为0.1%的甲酸)为流动相进行梯度洗脱;流速0.5 mL·min-1;柱温30 ℃;检测波长0~4.6 min,246 nm以及4.6~18 min,270 nm;通过对比保留时间和紫外吸收特征,结合峰纯度考察,对建立的指纹图谱中的主要特征峰进行准确指认,并归属组方中药来源;采用相似度软件,结合PCA以及PLS-DA方法,对16批市售产品进行质量评价。结果 建立了仙灵骨葆胶囊UPLC指纹图谱,对其中27个峰进行了化学指认和药材归属,相似度在0.959~0.988之间,造成相似度差异的化合物主要为来源于淫羊藿中的朝藿定C和补骨脂中的补骨脂酚、异补骨脂苷和补骨脂苷。结论 该方法专属性强,高效快速,可用于市售产品质量评价,为提升仙灵骨葆胶囊整体质量控制方法提供一定实验依据。
Abstract
OBJECTIVE To establish the ultra performance liquid chromatography(UPLC)fingerprint of Xianling Gubao Capsules (XLGB), and evaluate the product quality by chemometrics analysis method. METHODS The method was developed on an ACQUITY UPLC BEH Shield RP18 column (2.1 mm×50 mm, 1.7 μm) by gradient elution with acetonitrile-water [both containing 0.1% formic acid] as mobile phase at a flow rate of 0.5 mL·min-1. The column temperature was maintained at 30 ℃, and the detection wavelength was set at 246 nm during 0-4.6 min and 270 nm during 4.6-18 min. The main characteristic peaks were identified and assigned to individual herbs by comparing the retention time and UV absorption characteristics, combined with peak purity analysis. Furthermore, 16 batches of XLGB were evaluated by similarity assay, PCA, and PLS-DA. RESULTS The UPLC fingerprint of XLGB was established and 27 main characteristic peaks were identified. The similarity of 16 batches of XLGB was about 0.959 to 0.988, and epimedin C, bakuchiol, psoralenoside, and isopsoralenoside from Epimedium breviornu Maxim and Psoralea corylifolia L were the main compounds causing the similarity difference. CONCLUSION The method can be used for the quality control of XLGB with good specificity and efficiency, and this work provides the experimental basis to improve the overall quality control of XLGB.
关键词
仙灵骨葆胶囊 /
超高效液相色谱法 /
指纹图谱 /
质量评价
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Key words
Xianling Gubao Capsules /
ultra performance liquid chromatography /
fingerprint /
quality evaluation
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中图分类号：
R284
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脚注
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基金
十二五重大新药创制专项资助项目(2011ZX9201-201-05);广东省自然基金资助项目(S2013010012373)
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