[关键词]
[摘要]
目的 以高效液相色谱-二极管阵列检测器(HPLC-DAD)色谱图为基础建立地黄多波长指纹图谱,并通过熟地黄炮制终点检测分析其应用价值。方法 样品采用超声波法甲醇提取,蒸干后用15%甲醇定容,使用Waters Sunfire C18色谱柱(250 mm×4.6 mm,5 μm),乙腈-0.02%磷酸水溶液线性梯度洗脱,最大波长法选择多波长下重叠共有峰。用随机抽取的熟地样品多波长指纹图谱共有峰的平均值作为熟地的对照指纹图谱,通过炮制样品与熟地标准多波长指纹图谱的相似性比较获得最佳加工炮制时间。结果 结果显示205、284 nm下地黄多波长指纹图谱可获得18个共有峰。生地黄在蒸制25 h后与熟地黄对照指纹图谱相似性最大,是熟地黄蒸制的最佳时间。结论 多波长指纹图谱有利于显示样品成分细微变化及精确控制加工过程,可用于中药材加工过程中质量控制。
[Key word]
[Abstract]
Objective To develop the multi-wavelength chromatographic fingerprints for Rehmanniae Radix based on chromatographs of HPLC-DAD and to analyze the applicability by endpoint determination in processing Rehmanniae Radix Praeparae. Methods Samples were extracted by ultrasonic method with methanol. The extract solutions were evaporated to dry and the residue was dissolved with 15% methanol. A Waters Sunfire C18 column (250 mm × 4.6 mm, 5 μm) was applied. Acetonitrile-0.02% phosphoric acid in water was used as mobile phase for gradient linear eluting. Maximum peak area was the criterion for choosing from overlapping peaks of the same constituent under different wavelengths. The means of common peaks in the multi-wavelength chromatographic fingerprints of Rehmanniae Radix Praeparae chosen randomly were taken as the reference fingerprint index. The optimal processing time was determined by fingerprint similarity analysis between prepared samples and the reference. Results The result indicated that 18 common peaks were available in multi-wavelength chromatographic fingerprint under 205 and 284 nm. The similarity to reference Rehmanniae Radix Praeparae reached the summit after preparing for 25 h. It could be considered to be the optimum time for preparaing Rehmanniae Radix Praeparae. Conclusion The multi-wavelength chromatographic fingerprint is a facility for revealing constituents variations in detail and for accurate controlling the herbal medicine process.
[中图分类号]
[基金项目]
陕西省科技统筹项目(2012KTCL02-07);国家“十一五”科技支撑计划项目资助(2008BAD98B08)