反相高效液相色谱法测定决明降脂片中大黄素和大黄素甲醚的含量  

REVERSED PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR DETERMINATION OF EMODIN AND PHYSCION IN JUEMING JIANGZHI TABLETS

作　　者：律涛[1] 刘敏[2] 贾海红[2] 郎书会 樊淑彦[2] 

机构地区：[1]河北医科大学药学院实验中心,河北石家庄050017 [2]河北医科大学药学院分析化学教研室,河北石家庄050017

出　　处：《河北医科大学学报》2014年第8期908-910,共3页Journal of Hebei Medical University

摘　　要：目的：建立测定决明降脂片中大黄素和大黄素甲醚含量的反相高效液相色谱法（ reversed phase high performance liquid chromatography，RP-HPLC）。方法采用 RP-HPLC 测定大黄素和大黄素甲醚的含量。色谱柱为Kromasil C18色谱柱（250mm ±4.6mm，5μm）；流动相为甲醇-四氢呋喃-1％磷酸（84：7：9）；柱温为25℃；流速为1.0mL/ min；检测波长为254nm；进样量20μL。结果在选定的色谱条件下大黄素和大黄素甲醚的保留时间分别在6.9min、11.8min，具有良好的分离度和稳定性。大黄素回归方程为 Y ＝3.31±104 X -4.63±103（R ＝0.9997），进样量在3.12~9.4mg/ L 范围内与峰面积积分值呈良好线性关系，样品回收率为102.1％，相对标准差（ relative standard deviation，RSD）值为1.7％（n ＝9）；大黄素甲醚回归方程为 Y ＝2.35±104 X ＋8.80±103（R ＝0.9998），进样量在2.10-10.5mg/ L 范围内与峰面积积分值呈良好线性关系，样品回收率为104.7％，RSD 值为1.3％（n ＝9）。结论 RP-HPLC 操作可靠、准确，适用于决明降脂片中大黄素和大黄素甲醚的含量测定。Objective To establish a reversed phase high performance liquid chromatography （RP-HPLC）method for determination of emodin and physcion in Jueming Jiangzhi Tablets. Methods RP-HPLC system was carried out on Kromasil C18（250mm ± 4. 6mm,5μm）column with a mobile phase, the standards and samples were separated using a gradient mobile phase consisting of methanol, tetrahydrofuran and 1% phosphoric acid（84： 7： 9）. The column temperature was 25℃ and the flow rate was 1. 0mL/ min. The nuciferine was detected at the wavelength of 254 nm. The injection volume was 20μL. Results Emodin and physcion were separated from impurities well and its retention time was at about 6. 9 min,11. 8 min. Regress equation was Y = 3. 31 ± 104 X - 4. 63 ± 103（R = 0. 999 7）. The linear in the range of emodin was 3. 12 - 9. 36mg / L. The average recovery was 102. 1% ,and its RSD rate was 1. 7%（n = 9）;Regress equation was Y = 2. 35 ± 104 X ＋ 8. 80 ± 103（R = 0. 999 8）. The linear in the range of physcion was 2. 1 - 10. 5mg / L. The average recovery was 104. 7% ,and its RSD rate was 1. 3%（n = 9 ）. Conclusion RP-HPLC is areliable and accurate method,which can be applied for determination of emodin and physcion in Jueming Jiangzhi Tablets.

关 键 词：色谱法 高压液相 决明降脂片 大黄素 大黄素甲醛 

分 类 号：R446.1[医药卫生—诊断学] R975.3[医药卫生—临床医学]