作 者 ：李岑,肖远灿,杨红霞,杜玉枝,魏立新

期 刊 ：中国中药杂志 2011年 36卷 8期 页码：1046.

关键词：HPLC；当佐；没食子酸；羟基红花黄色素-A；桂皮醛；胡椒碱；

Keywords:HPLC, Dangzuo, gallic acid, hydroxysafflor yellow A, cinnamic aldehyde, piperine,

摘 要 ：目的: 建立HPLC同时测定藏药当佐中没食子酸、羟基红花黄色素-A、桂皮醛、胡椒碱含量的方法,对不同来源样品进行测定,以建立当佐的质量控制标准。 方法 :采用Waters XTerra RP-C₁₈(4.6 mm×250 mm,5 μm)色谱柱,以甲醇-水(含0.1 %冰乙酸)为流动相,梯度洗脱 (0~22.5 min,流动相比例5 ∶ 95~50 ∶ 50;22.5~40 min,流动相比例50 ∶ 50~80 ∶ 20),流速为1.0 mL·min^-1,检测波长为270 nm。 结果 :在此色谱条件下,没食子酸、羟基红花黄色素-A、桂皮醛、胡椒碱达到基线分离,且线性良好,线性范围分别为0.040~0.640 μg(r=0.999 8), 0.090~1.440 μg(r=0.999 9),0.031~0.500 μg(r=0.999 9), 0.092~1.477 μg (r=0.998 9),平均回收率(n=6)分别为97.42%(RSD 1.9%), 97.55 %(RSD 2.9%), 98.69%(RSD 0.96%), 96.72 %(RSD 4.0%);不同来源当佐中该4种成分的含量变化分别为0.113~1.69, 0.889~1.51, 0.000~0.606, 1.96~2.75 mg·g^-1。 结论 :本研究所建立的方法,能够准确快速地测定当佐中指标成分的含量,可为该药的全面质量评价提供参考。

Abstract:Objective : To develop an HPLC method for determination of gallic acid, hydroxysafflor yellow A, cinnamic aldehyde and piperine in Tibetan medicine Dangzuo, and to compare the content of four active components in Dangzuo of different Tibetan regions. Method : The separation was carried out on a Waters XTerra RP-C₁₈ column ( 4.6 mm×250 mm, 5 μm ). The mobile phases were methanol and water, all contained 0.1 % glacial acetic acid, for gradient elution. The gradient program was as follows: 0-22.5 min, methanol was changed from 5% to 50%; 22.5-40 min, changed to 80% 80 ∶ 20. The flow rate was 1.0 mL·min^-1. The detection wavelength was 270 nm. The reference wavelength was 500 nm. Result : The linear ranges of gallic acid, hydroxysafflor yellow A, cinnamic aldehyde and piperine were 0.040-0.640 μg ( r=0.999 8 ), 0.090-1.440 μg (r=0.999 9), 0.031-0.500 μg ( r=0.999 9 ) and 0.092-41.477 μg ( r=0.998 9), respectively. The average recoveries (n=6) were 97.42% (RSD 1.9%), 97.55%(RSD 2.9% ), 98.69% (RSD 0.96%) and 96.72% (RSD 4.0%), respectively. The content ranges of gallic acid, hydroxysafflor yellow A, cinnamic aldehyde and piperine in Dangzuo samples of different Tibetan regions were 0.113-41.69 mg·g^-1, 0.889-1.51 mg·g^-1, 0.000-40.606 mg·g^-1 and 1.96-2.73 mg·g^-1, respectively. Conclusion : The method is a simple and effective for quality control of Tibetan medicine Dangzuo.