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机构地区:[1]哈密地区药品检验所,哈密839000 [2]新疆医科大学第六附属医院,乌鲁木齐830000
出 处:《药物分析杂志》2017年第12期2191-2195,共5页Chinese Journal of Pharmaceutical Analysis
基 金:维吾尔药工艺及制剂关键技术研究与示范(项目编号2011030105-3)
摘 要:目的:建立RP-HPLC法同时测定复方消银颗粒中没食子酸、黄芩苷和黄芩素3个化学成分含量。方法:采用Shim-pack ODS(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~22 min,3%A→10%A;22~35 min,10%A→35%A;35~50 min,35%A→28%A),流速1.0 m L·min^(-1),检测波长为280 nm,柱温35℃。结果:没食子酸、黄芩苷和黄芩素质量浓度分别在3.57~49.98μg·m L^(-1)(r=0.999 5)、4.032~40.32μg·m L^(-1)(r=0.999 4)和3.278~16.390μg·m L^(-1)(r=0.999 3)范围内呈良好线性关系,平均回收率在98.74%~100.1%范围内,RSD在0.49%~1.5%范围内;3批样品中没食子酸、黄芩苷和黄芩素含量分别为0.153~0.154、0.256~0.258、0.113~0.114 mg·g^(-1)。结论:本方法可为复方消银颗粒多指标质量评价及控制提供科学依据。Objective:To establish an RP-HPLC method for simultaneous determination of three components ( gallic acid, baicalin and baicalein ) in compound Xiaoying granules. Methods: The samples were separated on a Shim-pack ODS column (250 mm·4.6mm, 5μm )by gradient elution with acetonitrile (A)-0.1% phosphoric acid aqueous solution ( B ) ( 0-22 min, 3%A → 10%A ; 22-35 min, 10%A →35%A ; 35-50 min, 35%A→28%A ) at a flow rate of 1.0 mL·min-1. The detection wavelength was set at 280 nm. The column temperature was maintained at 35℃. Results: The calibration curves of gallic acid, baicalin and baicalein were in good linearity over the ranges of 3.57-49.98μg·mL-1 ( r=0.999 5 ), 4.032-40.32μg·mL-1 ( r=0.999 4 ) and 3.278-16.390 μg·mL-1 ( r=0.999 3 ) , respectively ; their average recoveries were 98.74%- 100.1% with RSD values of 0.49%-1.5%. The contents of the above-mentioned compounds in samples were 0.153-0.154 mg·g-1, 0.256-0.258 mg·g-1 and 0.113-0.114mg·g-1, respectively. Conclusion: The method could be used for the comprehensive quality control of compound Xiaoying granules.
关 键 词:中医验方 复方消银颗粒 没食子酸 黄芩苷 黄芩素 反相高效液相色谱法
分 类 号:R917[医药卫生—药物分析学]
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