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作 者:杨鹏飞[1] 李保明[1] 王振中[2] 萧伟[2] 陈若芸[1]
机构地区:[1]中国医学科学院北京协和医学院药物研究所,天然药物活性物质与功能国家重点实验室,北京100050 [2]江苏康缘药业股份有限公司,江苏连云港222001
出 处:《中草药》2016年第18期3215-3218,共4页Chinese Traditional and Herbal Drugs
基 金:国家“十二五”科技重大专项(2012ZX09103201-043,2012ZX09301002-002)
摘 要:目的建立HPLC法同时测定桂枝茯苓胶囊(GFC)中4种茯苓三萜酸成分(去氢土莫酸、猪苓酸C、3-表去氢茯苓酸、去氢茯苓酸)的方法。方法色谱柱为Diamonsic C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.2%甲酸水溶液;梯度洗脱:0-70 min,50%-85%乙腈;70-80 min,85%-100%乙腈;80-90 min,100%乙腈;检测波长242 nm,体积流量1.0 m L/min,柱温40℃。结果去氢土莫酸、猪苓酸C、3-表去氢茯苓酸、去氢茯苓酸在HPLC中达到基线分离,线性范围分别为0.408-2.04(r=0.999 9)、0.192-0.96(r=0.999 5)、0.078-0.39(r=0.999 5)、0.075 6-0.378(r=0.999 5)μg/m L;平均加样回收率分别为97.5%、98.5%、97.2%、102.3%,RSD分别为1.4%、1.6%、1.2%、1.8%;测定了6批GFC,结果显示去氢土莫酸平均量为0.070 mg/粒,猪苓酸C平均量为0.015 mg/粒,3-表去氢茯苓酸平均量为0.030 mg/粒,去氢茯苓酸平均量为0.061 mg/粒。结论该方法可行、重现性好,可用于GFC的质量控制。Objective To establish an HPLC method for the determination of four triterpene constituents(dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid) in Guizhi Fuling Capsules(GFC). Methods Chromatography conditions were Diamonsic C18 column(250 mm × 4.6 mm, 5 μm), system mobile phase was composed of acetonitrile(A)-0.2% HCOOH aqueous solution(C) in a linear gradient elution mode(0—70 min: 50%—85% A; 70—80 min: 85%—100% A; 80—90 min: 100% A), detective wavelength was set at 242 nm, and column temperature was 40 ℃. Results The calibration curve was linear within 0.408—2.04 μg/m L(r = 0.999 9), 0.192—0.96 μg/m L(r = 0.999 5), 0.078—0.39 μg/m L(r = 0.999 5), and 0.075 6—0.378 μg/m L(r = 0.999 5) for dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid, respectively. The average recoveries were 97.5%(RSD = 1.4%, n = 5), 98.5%(RSD = 1.6%, n = 5), 97.2%(RSD = 1.2%, n = 5), and 102.3%(RSD = 1.8%, n = 5). Six batches of GFC sample were determined, The average contents of dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid were 0.070, 0.015, 0.030, and 0.061 mg/capsule, separately. Conclusion The method is simple, accurate, and can be used as a quality control method for GFC.
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