补肾强身胶囊中4种黄酮苷类成分的含量测定及转移率研究

Determination of four flavonoid glycosides in Bushen qiangshen Capsules and study on transfer rate

关键词:  补肾强身胶囊  高效液相色谱法  淫羊藿  黄酮苷  转移率  质量评价

Key words:  Bushen qiangshen capsules  HPLC  epimedii folium  flavonoid glycosides  transfer rate  quality control

摘要:

目的 建立HPLC同时测定补肾强身胶囊中4种黄酮苷类成分朝藿定A、朝藿定B、朝藿定C和淫羊藿苷的方法，并考察淫羊藿苷在工艺过程中的转移率。方法 采用50%乙醇超声提取，Agilent Zorbax SB-C₁₈（4.6 mm×250 mm，5 μm）分离，以乙腈-水为流动相，梯度洗脱，流速1.0 mL·min^–1，柱温40 ℃，检测波长为270 nm。结果 朝藿定A、朝藿定B、朝藿定C和淫羊藿苷在相应浓度范围内呈良好线性关系（r≥0.999），平均加样回收率分别为104.2%，103.2%，105.3%和103.7%，RSDs分别为1.4%，1.9%，0.9%和1.6%。9批自制成药中淫羊藿苷平均转移率为56.04%，计算确定补肾强身胶囊中淫羊藿苷含量限度应≥0.73 mg·g^–1，11个生产企业45批样品中有12批样品低于此限度，占比26.7%。结论 本方法重复性好，专属性强，简便易行，可用于补肾强身胶囊中淫羊藿的质量评价和转移率考察。

Abstract:

OBJECTIVE To determine 4 flavonoid glycosides of epimedin A, epimedin B, epimedin C, and icariin in Bushen qiangshen capsules by HPLC, and investigate the transfer rate of icariin from Epimedii Folium. METHODS After ultrasonic extracted by 50% ethanol, the sample was separated on an Agilent Zorbax SB-C₁₈ (4.6 mm×250 mm, 5 μm) column with the gradient elution. The mobile phase consisted of acetonitrile and water, with a flow rate of 1.0 mL·min^–1. The column temperature was set at 40 ℃, and the wavelength was set at 270 nm. RESULTS good linear relationships of epimedin A, epimedin B, epimedin C and icariin were obtained with correlation coefficients≥0.999. The average recoveries were 104.2%, 103.2%, 105.3% and 103.7%, and RSDs were 1.4%, 1.9%, 0.9% and 1.6%, respectively. The content limit of icarii was determined ≥0.73 mg·g^–1, with the average transfer rate of icariin from 9 batches of self-made samples as 56.04%. Among 45 batches of samples from 11 manufacturers, 12 batches were below the limit, indicative of a rate of 26.7%. CONCLUSION The method has good reproducibility and strong specificity, which is simple and easy, and can be used to inspect the transfer rate of icarii in the preparation process and improve the quality control.