忍冬藤饮片质量标准研究

Studies on the quality control of pieces of Rendongteng

目的制定忍冬藤饮片的质量控制方法。方法采用显微鉴别、薄层色谱定性鉴别,采用高效液相色谱法测定饮片中的马钱苷。色谱条件:苯基硅烷键合硅胶色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.4%磷酸溶液(12∶88),检测波长236 nm,流速1 m L·min-1,柱温40℃。结果非腺毛、木纤维、皮层纤维、表皮细胞、草酸钙簇晶、木化薄壁细胞等显微特征明显,显微鉴别方法专属性强;薄层色谱斑点清晰,阴性对照无干扰。马钱苷的进样量在0.086 8~1.302 0μg范围内与峰面积积分值呈良好的线性关系,相关系数r=0.999 9。平均回收率为99.96%,RSD=0.38%。测定山东、安徽、浙江等不同产地的19批样品,马钱苷含量以干燥品计算,结果在0.058%~0.863%区间分布。结论本方法准确可靠、重现性好,可有效控制该饮片的质量。

Objective To establish the quality standard of Rendongteng. Methods In the prescription,Rendongteng were identified qualitatively by TLC and microscope,and RP-HPLC was adopted to determine loganin. A phenyl silane bonded silica gel column（ 4.6 mm×250 mm,5 μm） was adopted with acetonitrile-0.4% phosphoric acid solution（ 12 ∶ 88） as mobile phase at a flow rate of 1 m L·min-1.The UV wavelength was set at 236 nm.The column temperature was 40 ℃.Results Microscopic characteristics such as nonglandular hairs,wood fiber,cortical fibers,epidermal cells,calcium oxalate crystal,wood parenchyma cells are obvious. The microscopic identification reflects a good specificity,TLC spots were clear and the black test showed no interference.The experiment showed good linear relationship at the ranges of 0.086 8 - 1.302 0μg（ r = 0.999 9）.In addition,the average recoveries were 99.96%（ RSD = 0.38%）.We had determined 19 batches of samples from Shandong,Anhui,Zhejiang and other different habitats.Conclusion The established method was accurate,reliable and reproducibility,can be used for the quality control of pieces of Rendongteng.