摘要
采用固相萃取净化处理,建立反相高效液相色谱测定强力定眩片中天麻素含量的方法,用于强力定眩片的质量控制。样品经SPE Pro Elut C18固相萃取小柱处理,采用Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱分离,以乙腈-0.1%冰醋酸(1∶99)为流动相,体积流量1.0 m L/min,柱温40℃,检测波长为220 nm。强力定眩片中天麻素含量测定的回归方程为y=27.945 4x+5.977 1,在1.31~104.80 mg/L范围内天麻素线性关系良好,相关系数为0.999 8,检出限为0.03 mg/L,低、中、高3个剂量的平均加样回收率为98.8%,RSD为1.2%,方法的重复性和精密度良好,符合含量测定方法要求。该法有效地消除了阴性干扰,专属性强,重现性好,快速准确,适用于强力定眩片中天麻素的测定。
To establish the determination method of gastrodin in Qianglidingxuan tablet by solid phase extraction and high performance liquid chromatography,samples were pretreated by SPE Pro Elut C18 solid phase column to remove lipid soluble substances and analyzed by high performance liquid chromatography consisting of a Diamonsil C18( 250 mm × 4. 6 mm,5 μm) column and a mixture of acetonitrile-0. 01% acetic acid( 1 ∶ 99) solution as the mobile phase. The detection wavelength was 220 nm,flow rate was1. 0 m L/min and column temperature was 40 °C. Gastrodin was well isolated. The determination of gastrodin in Qianglidingxuan tablets had the regression equation as y = 27. 9454 x + 5. 977 1. The calibration graph of gastrodin was linear within 1. 31 ~ 104. 80 mg/L( r = 0. 999 8). The detection limit of gastrodin was 0. 03 mg/L and the average recovery rate of low,medium and high doses was98. 8%( RSD was 1. 2%). This method shows good repeatability and accuracy,and meets the requirement of content determination method. The method can effectively eliminate the negative interference with good specificity,sensitivity and accuracy. It is suitable for the determination of gastrodin in Qianglidingxuan tablet.
作者
王颖
许蕾
WANG Ying;XU Lei(Xin Kanglong Pharmacy,the Fouth Affiliated Hospital of China Medical University,Shenyang 110032,China)
出处
《药物生物技术》
CAS
2018年第3期242-245,共4页
Pharmaceutical Biotechnology
关键词
强力定眩片
高效液相色谱法
天麻素
含量测定
质量控制
固相萃取
Qianglidingxuan tablet
HPLC
Gastrodin
Content determination
Quality control
Solid phase extraction