小茴香胶囊剂的制备工艺及有效成分含量测定研究

Study on Preparation Technology and Content Determination of Effective Components in Fennel Capsules

摘要: 目的：建立小茴香胶囊剂的制备工艺及其有效成分紫丁香苷(Syringin, SG)和槲皮素-3-O-β-D-葡萄糖醛酸苷(Quercetin-3-O-β-D-Glucuronide, QG)含量测定方法。方法：以流动性、吸湿性、成型性、辅料用量为考察指标筛选最佳辅料及用量，建立制剂工艺。通过堆密度测定，确定胶囊型号及装量。采用高效液相色谱法(High-Performance Liquid Chromatography, HPLC)测定胶囊剂中紫丁香苷和槲皮素-3-O-β-D-葡萄糖醛酸苷的含量。色谱柱：Agilent Eclipse XDB-C18 (250 mm × 4.6 mm, 5 μm)；流动相：乙腈和0.1%磷酸溶液二元梯度洗脱，流速1.0 mL/min，柱温30℃，检测波长245 nm，进样量10 μL。结果：原料粉与乳糖1:1混合均匀过筛，粘合剂选用25 mL/g的聚乙二醇，润滑剂选用2 mg/g硬脂酸镁，湿法制粒过20目筛制粒，平铺置于60℃烘箱中干燥30 min。罐装1号胶囊，装量规格为每粒0.2300 g，以SG和QG为对照品建立含量测定方法，测定小茴香胶囊内容物中SG含量为0.23%，QG含量为0.17%。结论：该制剂工艺稳定、可行；所建立的分析方法适用于SG和QG的含量测定。

Abstract: Objective: To establish the preparation technology of fennel capsules and the determination method of Syringin and Quercetin-3-O-β-D-Glucuronide. Methods: The fluidity, hygroscopicity, moldability, and dosage of excipients were used as indices to screen the best excipients and establish the preparation technology. Determine the capsule model and loading capacity through bulk density measurement. The contents of Syringin (SG) and Quercetin-3-O-β-D-Glucuronide (QG) in capsules were determined by high-performance liquid chromatography (HPLC). Chromatographic column: Agilent Eclipse XDB-C18 (250 mm × 4.6 mm, 5 μ m); Mobile phase: acetonitrile and 0.1% phosphoric acid solution were eluted by binary gradient, the flow rate was 1.0 mL/min, the column temperature was 30˚C, the detection wavelength was 245 nm, and the injection volume was 10 μ L. Results: The raw powder was mixed with lactose 1:1 and sieved evenly. The adhesive was 25 mL/g polyethylene glycol, and the lubricant was 2 mg/g magnesium stearate. The wet granulation was carried out through a 20-mesh sieve, and then it was laid flat in an oven at 60˚C for 30 min. Canned No.1 capsule, the loading specification is 0.2300 g per capsule, and the content determination method was established with SG and QG as reference substances. The content of SG and QG in the fennel capsule was determined to be 0.23% and 0.17%. Conclusion: The preparation process is stable and feasible. The established method is suitable for the determination of SG and QG.