目的 建立益心酮片高效液相色谱(HPLC)指纹图谱,并结合化学计量学分析方法比较全国范围内5家企业78批产品的质量差异。方法 采用HPLC建立360 nm波长下的指纹图谱,采用Agilent InfinityLab Poroshell 120EC-C18柱(4.6 mm×250 mm,4 μm),乙腈-四氢呋喃(A)和甲醇-0.5%甲酸(B)为流动相, 梯度洗脱(0～25min, 86%B→70%B; 25～27 min, 70%B; 27～28 min, 70%B→86%B; 28～30 min, 86%B);流速:0.7 mL·min-1;柱温:30 ℃;进样量:10 μL。并通过与对照品比较,确定特征峰及其归属。测定5家企业的78批产品,通过相似度评价,对不同批次益心酮片进行质量评价。结果 通过建立的78批益心酮片HPLC指纹图谱确证了8个共有峰,并对其中5个共有峰进行了指认;78批益心酮片的相似度均大于0.90,大部分样品相似度可达0.95以上。结论 益心酮片HPLC指纹图谱的构建为其质量控制提供了更加全面的参考依据,为科学评价及有效控制其质量提供了可靠方法。
Abstract
OBJECTIVE To establish the HPLC fingerprint of Yixintong tablets and compare the quality of 78 batches of Yixintong tablets from five enterprises in China. METHODS HPLC was used to establish fingerprint at 360 nm. Agilent infinity Lab Poroshell 120120EC-C18 column (4.6 mm×250 mm, 4 μm) was used. Acetonitrile- tetrahydrofuran (A)and methanol-0.5% formic acid (B)were used as mobile phase. Gradient elution was conducted(0-25 min, 86%B→70%B; 25-27 min, 70%B; 27-28 min, 70%B→86%B; 28-30min, 86%B); the flow rate was 0.7 mL·min-1; the column temperature was maintained at 30 ℃; the injection volume was 10 μL. By comparing with the reference substances, the characteristic peaks were determined. Then 78 batches of Yixintong tablets from five enterprises were determined, and the quality of different batches of products was evaluated by similarity evaluation. RESULTS Eight common peaks were determined by HPLC fingerprint of 78 batches of Yixintong tablets, and five of them were identified. The similarity of 78 batches of Yixintong tablets were all greater than 0.90, and most of them was more than 0.95. CONCLUSION The HPLC fingerprint of Yixintong tablets provides a more comprehensive reference for the quality control as well as a reliable method for the scientific evaluation and effective quality control.
关键词
益心酮片 /
指纹图谱 /
高效液相色谱法 /
质量评价
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Key words
Yixintong tablet /
fingerprint /
HPLC /
quality evaluation
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中图分类号：
R917
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参考文献
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脚注
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基金
国家十三五“重大新药创制”课题项目资助(2018ZX09735006); 中国食品药品检定研究院中青年基金项目资助(2020A3)
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