五味沙棘颗粒特征图谱及含量测定方法研究  

Study on characteristic fingerprint and quantitative analysis of Wuwei Shaji granules

作　　者：张华 刘俊萍 王菲菲 张海龙 张平平 

机构地区：[1]齐鲁医药学院药学教研室,淄博255213 [2]内蒙古宇航人药业有限责任公司,呼和浩特024000

出　　处：《药物分析杂志》2017年第9期1627-1632,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：山东省高等学校科技计划项目(J13LM57)

摘　　要：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 characteristic fingerprint of Wuwei Shaji granules and to determine gardenoside, liquiritin, isorhamnetin and glycyrrhizic acid in the preparation. Methods： C18 （ 4. 6 mm× 250 mm, 5 μm ） column was employed for chromatographic separation and the mobile phase was considered of acetonitrile and 0.1% phosphoric acid with a flow rate of 1.0 mL·min-1 with program elution： 0-25 min, 5%A → 19%A, 25-28 rain, 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. The column temperature was at 35 ℃ and the detection wavelength was set at 240 nm. Results： ＂Chinese medicine fingerprint similarity evaluation system 2004A＂ was used for the analysis and 22 common peaks were identified. Precision, stability and repeatability tests showed that RSD values of the relative retention times and the relative peak areas were all below 3.0%. Reference characteristic chromatogram was established and similarity evaluation was conducted. Four peaks were identified as characterized peaks of Fructus Hippophae, Glycyrrhizae Radix et Rhizoma and Gardeniae Fructus. Good linear correlations （r〉0.999 0）were found in the range of 0.058-0.134 mg· mL-1, 0.009-0.023 mg·mL-1, 0.006-0.014 mg· mL-1 and 0.030-0.070 mg· mL-1 for gardenoside, liquiritin, isorhamnetin and glycyrrhizic acid, respectively. Average recoveries were 99.5%, 100.2%, 100.3% and 98.3%, respectively. The content ranges of the 4 analytes were 1.05-1.19 mg· g-1, 0.15-0.21 mg· g-1, 0.18-0.45 mg·g-1and 0.30-0.36 mg· g-1. Conclusion： This study established characteristic chromatogram and multicomponent determination method for Wuwei Shaji granules, and provided reference for quality control of the drug.

关 键 词：五味沙棘方 达尔布班扎 栀子苷 甘草苷 异鼠李素 甘草酸 特征图谱 含量测定 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]