离心沉淀-天津中草药杂志社.PDF

中草药 Chinese Traditional and Herbal Drugs 第 42 卷 第 8 期 2011 年 8 月 ·1523 · 离心沉淀-离心超滤法测定盐酸青藤碱脂质体的包封率 郑杭生，佐拉 ·沙肯迪克，王湘林，徐莲英 上海中医药大学，上海 201203 摘 要：目的 建立盐酸青藤碱（sinomenine hydrochloride，SM-HCl ）脂质体包封率的测定方法，并阐明药物在脂质体中的 滞留特性。方法 采用薄膜分散法制备 SM-HCl 脂质体。以HPLC 法测定脂质体药物的量，色谱柱为 Kromasil ODS C18 柱（250 mm ×4.6 mm ，5 μm ），流动相为甲醇-水-乙二胺（55 ∶45 ∶0.225 ），体积流量 1.0 mL/min，检测波长265 nm 。以离心沉淀- 离心超滤法测定 SM-HCl 脂质体的包封率，并与以枸橼酸缓冲液（pH 7.0 ）水化的脂质体样品稀释前后的包封率进行对比。 结果 辅料与溶剂对青藤碱的定量测定无干扰，青藤碱在 9.82～78.56 μg/mL 线性关系良好（r ＝0.999 7 ），平均回收率在 99.29%～100.8%，日内与日间精密度良好（RSD ≤2.1% ）。50 μL 药液可使超滤膜对药物的吸附达到饱和。以枸橼酸缓冲液 （pH 7.0 ）水化的脂质体样品的包封率为33.16%，稀释 1 倍后该样品的包封率降至 14.75%。结论 HPLC 法与离心沉淀-离心 超滤法结合可用于测定 SM-HCl 脂质体的包封率，该方法快速、准确；离心超滤中应弃去 50 μL 初滤液以确保滤液与脂质体 外水相药物浓度一致；青藤碱与脂质双分子层有一定的亲和力，但在脂质体中的滞留性较差。 关键词：盐酸青藤碱脂质体；青藤碱；包封率；离心沉淀；离心超滤 中图分类号：R286.02 文献标志码：A 文章编号：0253 - 2670(2011)08 - 1523 - 05 Determination of entrapment efficiency of sinomenine hydrochloride liposomes with centrifugation sedimentation combined with centrifugation ultrafiltration ZHENG Hang-sheng, ZUOLA Shakendike, WANG Xiang-lin, XU Lian-ying Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China Abstract: Objective To develop a method for determining the entrapment efficiency of sinomenine hydrochloride (SM-HCl) liposomes and to illuminate the drug retention property in the liposomes. Methods Thin film hydration method was employed to prepare SM-HCl liposomes. HPLC was used to determine drug content of the liposomes. A Kromasil ODS C18 column (250 mm × 4.6 mm, 5 μm) was used with an isocratic elution composed of methanol, water, and ethylenediamine in the ratio of 55 : 45 : 0.225 at a flow rate of 1.0 mL/min. The column was maintained at 30 ℃. The UV detector was set at 265 nm. Centrifugation sedimentation combined with centrifugation ultrafiltration