中药女贞子饮片中8个成分的含量比较研究

Comparative study of the content of eight components in Ligustri Lucidi Fructus pieces

目的：针对不同来源女贞子和酒女贞子饮片中8个成分（红景天苷、酪醇、特女贞苷、木犀草苷、木犀草素、芹菜素、齐墩果酸、熊果酸）建立高效液相色谱含量测定方法,并对女贞子、酒女贞子饮片及水煎煮前后所测成分的含量进行比较,为其质量标准提高和临床应用提供依据。方法：采用液相色谱法,使用Agilent Prep-C18（4.6 mm×250 mm,5μm）色谱柱,以乙腈（A）-0.02%磷酸水溶液（B）为流动相,梯度洗脱（0~5 min,5%A→10%A;5~15 min,10%A;15~60 min,10%A→33%A;60~65 min,33%A→90%A;65~75 min,90%A;75~80 min,100%A）,流速1 m L·min-1,检测波长224 nm（测定红景天苷、酪醇、特女贞苷）、349 nm（测定木犀草苷、木犀草素、芹菜素）、206 nm（测定齐墩果酸、熊果酸）,柱温25℃。结果：建立的8个成分含量测定方法简便、可行;女贞子、酒女贞子饮片中红景天苷、酪醇、木犀草素和芹菜素的含量存在显著性差异;2种饮片的水煎液中红景天苷、酪醇、特女贞苷、木犀草苷可检出,且变化明显。结论：木犀草素和芹菜素可以用于饮片的鉴别,红景天苷、酪醇、特女贞苷、木犀草苷具有特征性,可用于女贞子、酒女贞子饮片的质量评价。

Objective：To establish an HPLC method for determination of eight components （salidroside, tyrosol, specnuezhenide, luteolin-7-O-glucoside, luteolin, apigenin, oleanolic acid and ursolic acid） in Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces from different sources, and compare the content in the water decoction, Ligustri Lucidi Fructus, so as to provide a foundation for the improvement of quality standard and clinical application. Methods： The analysis was performed on an Agilent Prep-C 18 （4- 6 mm ×250 mm ,5 μm）column. The mobile phase was acetonitrile （ A）-O. 02% phosphoric acid aqueous （ B ） with gradient elution mode （ 0-5 min, 5 % A→10% A ;5-15 min, 10% A ; 15-60 min, 10%→33 % A ;60-65 min, 33 % A→90% A ;65-75 min, 90% A ;75-80 min, 100% A） , at a flow rate of 1 mL . min-1. The detection was set at 224 nm for salidroside,tyrosol,and specnuezhenide ;349 nm for luteolin-7-O-glucoside, luteolin, and apigenin ; 206 nm for oleanolic acid and ursolic acid. The column temperature was controlled at 25 ℃. Results： The HPLC determination method established for eight components is easy and feasible;the content of salidroside, tyrosol, luteolin and apigenin were significantly different between Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieees;salidroside, tyrosol, specnuezhenide and luteolin-7-O-glucoside could be detected and obviously changed in the water decoction of two kinds of pieces. Conclusion ： Luteolin and apigenin can be used for identification of two pieces. Salidroside, tyrosol, speenuezhenide and luteolin-7-O-glucoside are characteristic. The HPLC determination method established in the study can be used for the quality control of Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces.