[关键词]
[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,5 μm),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 mL/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/mL;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。
[Key word]
[Abstract]
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/mL(r=0.999 9),0.192-0.96 μg/mL(r=0.999 5),0.078-0.39 μg/mL(r=0.999 5),and 0.075 6-0.378 μg/mL(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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[基金项目]
国家“十二五”科技重大专项(2012ZX09103201-043,2012ZX09301002-002)