HPLC法同时测定当归片中阿魏酸、洋川芎内酯Ⅰ和藁本内酯的含量  

Simultaneous determination of ferulic acid,senkyunolide Ⅰ and ligustilide for Danggui Tablets by HPLC

作　　者：叶晓娅 薛晓会 YE Xiaoya;XUE Xiaohui(Pingdingshan Institute for Food and Drug Control,Pingdingshan 467000,China)

机构地区：[1]平顶山市食品药品检验所,平顶山467000

出　　处：《中国药品标准》2018年第4期295-298,共4页Drug Standards of China

摘　　要：目的:同时测定当归片中阿魏酸、洋川芎内酯Ⅰ和藁本内酯的含量。方法:采用Ultimate XB-C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈-水为流动相,梯度洗脱;检测波长为280 nm;流速为1.0 m L·min^(-1);进样量为10μL;柱温为30℃。结果:阿魏酸、洋川芎内酯Ⅰ和藁本内酯的线性范围分别为0.021 46~0.214 6μg(r=0.999 0)、0.036 22~0.362 2μg(r=1.000 0)、0.089 42~0.894 2μg(r=1.000 0);提取回收率分别为97.1%(RSD为2.3%,n=6)、103.2%(RSD为1.4%,n=6)和98.2%(RSD为1.0%,n=6),测定了三批样品,3个成分的测定结果分别为:批号170503:0.461、0.236、0.907 mg·片^(-1);批号170820:0.508、0.267、0.937 mg·片^(-1);批号171206:0.482、0.245、0.892 mg·片^(-1)。结论:本法经方法学考察均符合有关规定,可用于当归片的质量控制。Objective： To establish a method for simultaneous determination of ferulic acid,senkyunolide I and ligustilide in Danggui Tablets. Methods： The test was performed in Ultimate XB-C18 column（ 4. 6 mm × 250 mm,5 μm） under the gradient elution of acetonitrile-water. The detection wavelength was 280 nm,the flow rate was 1. 0 ml·min^-1,the injection volume was 10 μL,and the column temperature was 30 ℃. Results：The linearity ranges of ferulic acid,senkyunolide Ⅰ and ligustilide fell into 0. 021 46-0. 214 6 μg（ r = 0. 9990）,0. 036 22-0. 362 2 μg（ r = 1. 000 0）,and 0. 089 42-0. 894 2 μg（ r = 1. 000 0） respectively. The average recoveries of ferulic acid,senkyunolide I and ligustilide were 97. 1 % with RSD as 2. 3 %（ n = 6）,103. 2 % with RSD as 1. 4 %（ n = 6）,and 98. 2 % with RSD as 1. 0 %（ n = 6） respectively. The test results of ferulic acid,senkyunolide Ⅰ and ligustilide in 3 batches of samples were respectively as follow： lot No.170503 ： 0. 461,0. 236,0. 907 mg per tablet; lot No. 170820 ： 0. 508,0. 267,0. 937 mg per tablet; lot No. 171206 ： 0. 482,0. 245,0. 892 mg per tablet. Conclusion： The methodology validation results meet the relevant requirements,and show that this established method can be used for the quality control of Danggui Tablets.

关 键 词：当归片 含量测定 阿魏酸 洋川芎内酯Ⅰ 藁本内酯 HPLC 

分 类 号：R921.2[医药卫生—药学]