甘遂半夏汤的UPLC—DAD指纹图谱研究
超高效液相色谱,质量控制
洪博 刘军 张杰 徐天娇 王玉春 李文静中图分类号 R917 文献标志码 A 文章编号 1001-0408(2018)17-2373-04
DOI 10.6039/j.issn.1001-0408.2018.17.16
摘 要 目的:建立甘遂半夏汤的指纹图谱,为完善其质量控制提供参考。方法:采用超高效液相色谱-二极管阵列检测器(UPLC-DAD)法建立13批甘遂半夏汤的指纹图谱,色谱柱为Waters Acquity UPLC HSS T3,流动相为0.1%甲酸-乙腈(梯度洗脱),流速为0.5 mL/min,检测波长为254 nm,柱温为35 ℃,进样量为4 μL。采用《中药色谱指纹图谱相似度评价系统》(2004A版)对指纹图谱进行评价,并采用SPSS 13.0软件对各样品进行聚类分析。结果:方法学考察中,各色谱峰的保留时间和相对峰面积的RSD均小于2%(n=6)。13批甘遂半夏汤指纹图谱的相似度均大于0.95,确定了21个共有色谱峰,并指认了其中芍药苷、甘草苷及甘草酸3个共有色谱峰。聚类分析结果显示,甘遂半夏汤样品分为2类。结论:建立的UPLC-DAD指纹图谱体现了甘遂半夏汤组分的整体特征,为甘遂半夏汤制剂质量标准的建立提供了可靠依据。
关键词 甘遂半夏汤;超高效液相色谱-二极管阵列检测器法;指纹图谱;质量控制
ABSTRACT OBJECTIVE: To establish the fingerprints of Gansui banxia decoction, and to provide reference for improving quality control. METHODS: UPLC-DAD was used to establish the fingerprints of 13 batches of Gansui banxia decoction. The determination was performed on Waters Acquity UPLC HSS T3 column with mobile phase consisted of 0.1% formic acid- acetonitrile (gradient elution) at the flow rate of 0.5 mL/min. The detection wavelength was set at 254 nm, and column temperature was 35 ℃. The sample size was 4 μL. Similarity Evaluation System for Chromatographic Fingerprint of TCM (2004A edition) was used to evaluate the fingerprints. SPSS 13.0 software was used for cluster analysis of those samples. RESULTS: In the methodology validation ......
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