摘要
目的:建立同时测定复方一枝蒿速释微丸中(R,S)-告依春、一枝蒿酮酸、靛玉红3种化学成分含量的高效液相色谱方法。方法:采用Shim-pack ODS色谱柱(250 mm×4.6mm,5μm),流动相为乙腈(A)-0.5%磷酸水溶液(B),梯度洗脱(0~15 min,3%A→10%A;15~20 min,10%A→35%A;20~35 min,35%A),检测波长为245 nm(0-20 min,检测(R,S)-告依春)和289 nm(25-35 min,检测靛玉红和一枝蒿酮酸),流速1.0 mL·min^(-1),柱温30℃。结果(R,S)-告依春、靛玉红、一枝蒿酮酸质量浓度分别在3.904~54.656μg·mL^(-1)(r=0.999 5)、3.064-42.896μg·mL^(-1)(r=0.999 3)和7.264-101.696μg·mL^(-1)(r=0.999 6)范围内呈良好线性关系;复方一枝蒿速释微丸中3种有效成分的平均回收率(n=3)分别为99.27%~100.14%(RSD<1.2%),99.16%~99.72%(RSD<1.4%),99.39%~99.81%(RSD<1.7%)。3批样品中(R,S)-告依春、靛玉红、一枝蒿酮酸3个成分的含量测定结果分别为0.343 5-0.3501、0.1907-0.199 9、0.887 2-0.895 6mg·g^(-1)。结论:方法学验证结果表明,本法可为复方一枝蒿速释微丸多指标质量评价及控制提供科学依据。
Objective： To establish an HPLC method for simultaneous detemination of three components [ （ R, S ） -epigoitrin, rupestonic acid and indirubin I in the effective fraction of compound Yizhihao immediate-release pellets. Method ： The samples were separated on a Shim-pack ODS column （ 250 mm×4.6mm, 5μm ） by gradient elution at a flow rate of 1.0 mL·min-1. The mobile phase consisted of acetonitrile （ A ） -0.5% phosphoric acid aqeous solution（ B ） （ 0-15 rain, 3%A→10%A; 15-20 min, 10%A→ 35%A; 20-35 min, 35%A ）. The detection wavelength was set at 245 nm（ 0-20min ）for（R, S）-epigoitrin and 289 nm（ 25-35 rain ） for indirubin and rupestonic acid. The column temperature was maintained at 30℃. Results： The calibration curves of（ R, S ）-epigoitrin, rupestonic acid and indirubin were in good linearity within the ranges of 3.904-54.656μg· mL-1 （ r=0.999 5 ） , 3.064-42.896μg· mL-1 （ r=0.999 3 ） , 7.264-101.696 μg· mL-1（ r=0.999 6 ）respectively. The average recoveries （ n=3 ） were 99.27%- 100.14% with RSD〈 1.2%, 99.16%-99.72% with RSD〈 1.4%, and 99.39%-99.81% with RSD〈1.7%. The eontents in 3 samples were in the ranges of 0.343 5-0.350 1 mg· g-1 for（ R,S ） - epigoitrin, 0.190 7-0.199 9 mg· g-1 for indirubin, and 0.887 2-0.895 6 mg· g-1 for rupestonic acid. Conclusion： The resuhs of methodology validation show that the established method can be used for the comprehensive quality control of compound Yizhihao immediate-release pellets.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第1期142-147,共6页
Chinese Journal of Pharmaceutical Analysis
基金
新疆维吾尔自治区乌鲁木齐市科学技术项目(项目编号Y151310010)
关键词
复方一枝蒿速释微丸
板蓝根
大青叶
一枝蒿
(R
S)-告依春
一枝蒿酮酸
靛玉红
高效液相色谱法
compound Yizhihao immediate-release pellets
Radix Isatidis
Isatidis Folium
Herba ArtemisiaeRupestridis
（ R, S ）-epigoitrin
rupestonic acid
indirubin
HPLC
