摘要
目的:建立同时测定健脑合剂中大黄素和齐墩果酸含量的高效液相色谱方法。方法:采用Thermo ODS-2 HYPERSILC_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为0.1%醋酸水溶液(A)-甲醇(B),线性梯度洗脱[0～10 min,40%B～90%B;10～30 min,90%B],流速1.0 ml·min^(-1);柱温为35℃;检测波长分别为254 nm(大黄素),208 nm(齐墩果酸)。结果:大黄素和齐墩果酸的浓度分别在0.11～214.80μg·ml^(-1)和0.85～854.40μg·ml^(-1)范围内均呈良好线性关系(r≥0.999 4);日内、日间精密度良好,RSD≤1.89%(n=6);各组分低、中、高浓度的平均加样回收率98.50%～99.62%,RSD≤1.85%(n=18);健脑合剂中大黄素和齐墩果酸的浓度分别为(10.68±0.18)μg·ml^(-1)和(29.80±0.32)μg·ml^(-1)。结论:本方法简便可靠、专属性强、重复性好,适用于健脑合剂质量控制。
Objective： To develop an HPLC method for the simultaneous determination of emodin and oleanolic acid in Jiannao mixtures. Method： A Thermo ODS-2 HYPERSIL Cls column （250 mm × 4. 6 mm,5 um） was used. The mobile phase consisted of 0. 1% aqueous acetic acid （A） and methanol （B） with linear gradient elution （0-10 min,40%-90% B;10-30 min ,90% B）. The flow rate was 1.0 ml. min- 1. DAD detection was used and the detection wavelength was set at 254 nm for emodin and 208 nm for oleanolic acid. The column temperature was 35 ℃. Result： Emodin and oleanolic acid showed good linearity （r≥ 0. 999 4） within the range of 0. 11-214. 80 p,g. mI- ~ and 0. 85-854.40 ug· ml-1 , respectively. The RSDs of intra-and inter-day precisions were below 1.89% （ n = 6）. The average recoveries of the two investigated compounds at low, medium and high concentration levels were within the range of 98. 50%-99.62% with RSDs below 1.85% （ n = 6）. The conten（ of emodin and oleanolic acid in Jiannao mixtures were （ 10. 68 ± 0. 18 ） ug· ml - 1 and （29. 80 ± 0. 32） ug- ml - 1, respectively. Conclusion ： The developed method is simple, accurate and reliable, and can be used for the quality control of Jiannao mixtures.
出处
《中国药师》
CAS
2012年第1期61-63,共3页
China Pharmacist
