摘要
目的建立丹参药材水溶性成分中丹参素、原儿茶醛、丹酚酸B和脂溶性成分中二氢丹参酮I、隐丹参酮、丹参酮I、丹参酮IIA的含量测定方法。方法采用高效液相色谱法测定,色谱柱为汉邦C18色谱柱(4.6 mm×250 mm,5μm);流动相A为0.1%甲酸-水(V/V),流动相B为乙腈,线性洗脱梯度为0～10 min,B相10%～20%,10～27 min,B相20%～33%,27～30 min,B相33%～70%,30～50 min,B相70%～85%;柱温:20℃;流速:1 mL.min-1;进样量:10μL;检测波长:280 nm。结果丹参素、原儿茶醛、丹酚酸B、二氢丹参酮I、隐丹参酮、丹参酮I和丹参酮IIA在0.037 2～118.000 0,0.017 4～8.900 0,0.141～450.000,0.018 8～56.800 0,0.049 7～158.000 0,0.021 5～78.500 0,0.096 2～308.000 0 mg.L-1浓度范围内均呈良好线性关系(R2≥0.999 2);各成分的平均加样回收率均在98.5%～101.5%,RSD均<1.98%(n=6);日内日间精密度良好,RSD均<2.16%。结论该方法简便、准确、重复性好,可用于丹参药材的含量测定。
Objective To establish a method for determination of the hydrophilic of danshensu, protocatechuic aldehyde, salvianolic acid B and lipophilic compounds of dihydro-tanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone ⅡA in Radix Salviae Miltiorrhizae. Methods Chromatography was performed on a Lichrospher-C18 column （250 mm × 4.6 mm i. d. ; 5 μm particle size）. The separation was achieved by a linear gradient elution. Mobile phase was the mixture of solvent A （ 1% aqueous formic acid） and solvent B （acetonitrile）. The gradient elution was conducted as follows： 10% -20% B in 0 - 10 min, 20% - 33% B in 10 -27 min, 33% -70% B in 27 -30 min, and 70% -85% B in 30 -50 min. The injection volume of 10 μL and the UV wavelength of 280 mn were used in the analysis. The flow rate was 1.0 mL · min^-1 and the column operated at 20 ℃. Results A good linearity was obtained with the correlation coefficients of tanshinol, protocatechualdehyde, salvianolic acid B, dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone ⅡA ranged from 0. 037 2 - 118. 000 0 mg ·L^-1, 0. 017 4 - 8.900 0 mg·L^-1 , 0. 141 -450. 000 mg ·L^-1 , 0. 018 8 -56. 800 0 mg ·L^-1 , 0.049 7 - 158. 000 0 mg·L^-1 , 0. 021 5 - 78. 500 0 mg ·L^-1, 0.096 2-308. 000 0 mg·L^-1 （ R^2 ≥0. 999 2 ）, respectively. The average recovery rates of the four investigated compounds were in the range of 98.5% - 101.5% for all with RSD below 1.98% （ n = 6）. The intra-day and inter-day precision of the assay were no more than 2.16% （n = 6）. Conclusion The method is accurate and reliable with good reproducibility, and can be used as a determination standard for Radix Salviae Miltiorrhizae.
出处
《医药导报》
CAS
2009年第10期1345-1348,共4页
Herald of Medicine
基金
国家重点基础研究发展计划(973计划)项目(基金编号:2005CB523402)
关键词
丹参
丹参素
丹酚酸B
二氢丹参酮I
色谱法
高效液相
Radix Salviae Miltiorrhizae
Danshensu
Salvianolic acid B
Dihydro-tanshinone Ⅰ
HPLC
