高效液相色谱-蒸发光散射检测法测定中药及制剂中齐墩果酸和熊果酸的含量  被引量:14

HPLC - ELSD Determination of Oleanolic Acid and Ursolic Acid in Chinese Herbal Medicine and Chinese Patent Medicines

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作  者:赵宇新[1] 李曼玲[1] 

机构地区:[1]中国中医研究院中药研究所,北京100700

出  处:《药物分析杂志》2004年第2期167-170,共4页Chinese Journal of Pharmaceutical Analysis

摘  要:目的:建立高效液相色谱-蒸发光散射检测法测定中药饮片及中成药制剂中齐墩果酸和熊果酸的含量。方法:采用Kromasil C18(4.6 mm×250 mm,5μm)色谱柱,柱温40℃;甲醇-水-冰醋酸(260:40:0.15)为流动相,流速0.6 mL·min-1;蒸发光散射检测器检测,漂移管温度85℃,气体流速2.60 L·min-1。结果:齐墩果酸在0.562-2.81μg范围内(r=0.9998),熊果酸在0.380-1.90μg范围内(r=0.9996)线性关系良好。药材(木瓜)中齐墩果酸和熊果酸的回收率分别为98.2%和99.8%,RSD(n=5)分别为3.2%和3.4%。中成药制剂(知柏地黄丸)中齐墩果酸和熊果酸的回收率分别为100.0%和100.1%,RSD(n=5)分别为2.1%和2.9%。结论:方法简便、准确,重现性好。Objective: To establish a method for the determination of oleanolic acid and ursolic acid in Chinese herbal medicine and Chinese patent medicines. Method:Chromatography was performed on a 5 μn Kromasil C18 column(4. 6 mm×150 mm) at 40℃. The mobile phase composition was methanol - water - acetic acid(260: 40 :0.15) with a flow rate of 0. 6 m·min -1. An evaporative light - scattering detector( ELSD) was used as detector with gas flow rate of 2. 60 L·min -1 and drift tube temperature of 85℃. Results: The oleanolic acid has a good linearity relationship(r= 0.9998,n=5 ) between 0.562-2. 81μg. The ursolic acid has a linear range between 0. 380 -1. 90μg with r = 0. 9996 ( n = 5 ) . Average recovery of oleanolic acid in Chinese herbal medicine was 98. 2% with RSD of 3. 2% ;the ursolic acid was 99. 8% with RSD of 3. 4% . The average recovery of two constituents in Chinese patent medicines was 100. 0% (RSD =2.1%)and 100. 1 % ( RSD = 2. 9% )respectively. Conclusion: It was proved that the method was reliable, simple and accurate.

关 键 词:高效液相色谱-蒸发光散射检测法 中药 齐墩果酸 熊果酸 含量测定 质量控制 

分 类 号:R286.0[医药卫生—中药学]

 

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