贞苓增免散的质量标准研究

Study on the quality standard of Zhenling Zengmian powder

通过对贞苓增免散进行定性鉴别、定量分析,建立该制剂的质量控制方法。本研究采用薄层色谱法对女贞子、茯苓进行定性鉴别;采用高效液相色谱法测定贞苓增免散中特女贞苷的含量,条件为:以十八烷基硅烷键合硅胶为填充剂、甲醇-水(40:60)为流动相、检测波长224 nm、流速1.0 mL/min、柱温室温、进样量10μL;同时采用硫酸-蒽酮法测定贞苓增免散中茯苓多糖的含量,以葡萄糖为对照品,硫酸-蒽酮溶液为显色剂,在620 nm处测定OD值。结果显示:薄层色谱斑点清晰、无阴性干扰、专属性强、分离度高,能有效鉴别女贞子、茯苓;加样回收试验测得特女贞苷与茯苓多糖的含量分别在0.03~0.30 g/L、0.052~0.100 g/L呈良好的线性关系,平均加样回收率分别为98.28%、99.20%,RSD分别为2.17%、2.22%;高效液相法测得贞苓增免散中特女贞苷含量为12.3 mg/g;硫酸-蒽酮法测得0.1 g/L中贞苓增免散中茯苓多糖含量为0.077 8 mg。本研究建立的方法简便易行、稳定性、重复性好,可有效控制贞苓增免散的质量。

Through the qualitative identification and quantitative analysis of Zhenling Zengmian powder, the quality control method of the preparation was established. In the study, Ligustrum lucidum and Poria cocos were qualitatively identified by TLC, and the content of Ligustrin in Zhenling Zengmian powder was determined by HPLC as follows: octadecyl silane bonded silica gel was used as filler, methanol-water(40:60) was used as mobile phase, detection wavelength was 224 nm, flow rate 1.0 mL/min, column temperature room temperature, injection volume 10 μL. At the same time, sulfuric acid-anthrone method was used to determine the content of Poria cocos polysaccharide in Zhenling Zengmian powder. With glucose as the control substance and sulfuric acid-anthrone solution as the chromogenic agent, the OD value was determined at 620 nm. The results showed that: TLC had clear spots,no negative interference, strong specificity and high separation, and could effectively identify Ligustrum lucidum and Poria cocos. The sample recovery experiment showed that the content of Ligustrin and pachymaran showed a good linear relationship in 0.03~0.30 g/L and 0.052~0.100 g/L, and the average recovery rates were 98.28% and 99.20%, respectively, and the RSDs were 2.17% and 2.22%, respectively. The content of Ligustrin in Zhenling Zengmian powder was 12.3 mg/g determined by HPLC. The content of Poria cocos polysaccharide in Zhenling Zengmian powder in 0.1 g/L was determined to be 0.077 8 mg by sulfuric acid-anthrone method. The method established in the study is simple, stable and reproducible, and can effectively control the quality of Zhenling Zengmian powder.