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目的:建立五味沙棘颗粒的特征图谱,并对栀子苷、甘草苷、异鼠李素、甘草酸进行定量研究。方法:采用C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈为流动相A,0.1%磷酸水溶液为流动相B,梯度洗脱(0~25 min,5%A→19%A;25~28 min,19%A→23%A;28~34 min,23%A→26%A;34~40 min,26%A→32%A;40~65 min,32%A→58%A),流速1 mL·min~(-1),柱温35℃,检测波长240 nm。结果:采用《中药色谱指纹图谱相似度评价系统2004A版》进行分析,建立了以甘草苷为参照峰的五味沙棘颗粒HPLC特征图谱,确定了22个共有峰,精密度、稳定性和重复性试验中各共有峰相对保留时间和相对峰面积的RSD均小于3.0%。建立了五味沙棘颗粒的对照特征图谱,并进行相似度分析,归属了4个特征峰作为沙棘、栀子、甘草3味药材的特征峰。特征图谱中栀子苷、甘草苷、异鼠李素、甘草酸质量浓度分别在0.058~0.134、0.009~0.023、0.006~0.014、0.030~0.070 mg·mL~(-1)范围内线性关系良好(r>0.999 0),平均回收率分别为99.5%、100.2%、100.3%、98.3%。外标法测定栀子苷、甘草苷、异鼠李素和甘草酸含量分别在1.05~1.19、0.15~0.21、0.18~0.45和0.30~0.36 mg·g~(-1)范围内。结论:本研究建立了五味沙棘颗粒特征图谱及多指标成分含量测定的方法,为五味沙棘颗粒的质量控制提供了依据。
OBJECTIVE: To establish the characteristic map of Seabuckthorn granules, and to quantitatively study geniposide, liquiritin, isorhamnetin and glycyrrhizin. METHODS: The mobile phase B was eluted with C 18 column (4.6 mm × 250 mm, 5 μm) using acetonitrile as mobile phase A and 0.1% phosphoric acid as mobile phase B (0-25 min, 5% A → 19% A; 25-28 min, 19% A → 23% A; 28-34 min, 23% A → 26% A; 34-40 min, 26% A → 32% A; 40-65 min, 32% A → 58% A), flow rate 1 mL · min ~ (-1), column temperature 35 ℃, detection wavelength 240 nm. Results: The chromatographic fingerprint chromatogram of Chinese medicine Chromatographic Fingerprinting System 2004A was used to analyze the HPLC characteristic map of Seabuckthorn Seabuckthorn with the reference peak of liquiritin, and 22 common peaks, precision, stability and repeatability were determined The RSDs of the relative retention time and the relative peak area of each common peak were less than 3.0%. The characteristic map of the seabuckthorn granules was established and the similarity analysis was carried out. Four characteristic peaks were assigned as the characteristic peaks of the three medicinal materials of seabuckthorn, gardenia and licorice. The chromatograms of geniposide, liquiritin, isorhamnetin and glycyrrhizin showed good linearity in the range of 0.058 ~ 0.134, 0.009 ~ 0.023, 0.005 ~ 0.014 and 0.030 ~ 0.070 mg · mL ~ (-1) r> 0.999 0). The average recoveries were 99.5%, 100.2%, 100.3% and 98.3%, respectively. The contents of geniposide, liquiritin, isorhamnetin and glycyrrhizic acid in the external standard method were 1.05-1.19, 0.15-0.21, 0.18-0.45 and 0.30-0.36 mg · g -1, respectively. Conclusion: This study established a method for determining the characteristic map of Fructus Schisandrae and the content of multi-index components of Fructus schisandrae, which provided the basis for the quality control of Fructus Schisandrae.