目的 将对照制剂引入牛黄清胃丸的指纹图谱研究,对样品的质量等级进行初评价。方法 采用超高效液相色谱法,色谱柱为AQUITY UPLC BEH C18柱,流动相为乙腈(含0.5%甲酸)-0.5%甲酸梯度洗脱,流速为0.2 mL·min-1,进样量2 μL,柱温40 ℃,检测波长254 nm。与对照品和对照药材比较,确定特征峰及其归属。以牛黄清胃丸对照制剂为随行实物对照,计算18个厂家49批样品指纹图谱的相似度,并对其质量等级进行初评价。结果 样品相似度在0.76～0.98之间,49批相似度大于0.75,达到二等限度,24批样品相似度大于0.90,达到一等限度。结论 所建方法简便、准确、快速,可用于牛黄清胃丸的质量控制和等级评价,也可为中成药的质量等级研究提供参考。
Abstract
OBJECTIVE To apply reference drug in the fingerprint study of Niuhuang qingwei pills, and perform primary evaluation of the quality grade of the samples. METHODS Ultra performance liquid chromatography (UPLC) separation was performed on an AQUITY UPLC BEH C18 column with gradient elution using acetonitrile (containing 0.5% formic acid)-0.5% formic acid at a flow rate of 0.2 mL·min-1. The injection volume was 2 μL and the column temperature was maintained at 40 ℃. The detection wavelength was set at 254 nm. By comparing with reference substances and the reference herbal materials, characteristic peaks and their ascriptions were investigated. Using Niuhuang qingwei pills reference drug as the accompanying physical control, the similarities of the fingerprints of 49 batches of samples from 18 manufacturers were calculated, and the quality grades were evaluated. RESULTS The similarities of all samples fell within the range of 0.76-0.98. The similarities of 49 samples were above 0.75 and met the second-grade limit. The similarity of 24 samples were above 0.90 and met the first-grade limit. CONCLUSION The method is simple, accurate and rapid. It can be used for the quality control and grade evaluation of Niuhuang qingwei pills, which provides reference for the quality grade research of Chinese patent medicines.
关键词
牛黄清胃丸 /
对照制剂 /
质量等级 /
指纹图谱 /
超高效液相色谱法
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Key words
Niuhuang qingwei pills /
reference drug /
quality grade /
fingerprint /
ultra performance liquid chromatography (UPLC)
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中图分类号：
R917
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参考文献
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