红荷山葡降脂胶囊制备工艺及含量测定方法研究  

Preparation Process and Content Determination Method of Hongheshanpu Lipid-Lowering Capsules

作　　者：孙思琪 李想 刘晓云 任雪阳 王宇 董英 马嘉慕 宋若兰 范琦琦 魏静 于啊香 王秀环 折改梅[1] SUN Siqi;LI Xiang;LIU Xiaoyun;REN Xueyang;WANG Yu;DONG Ying;MA Jiamu;SONG Ruolan;FAN Qiqi;WEI Jing;YU Axiang;WANG Xiuhuan;SHE Gaimei(School of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing,China 102488)

机构地区：[1]北京中医药大学中药学院,北京102488

出　　处：《中国药业》2021年第19期34-38,共5页China Pharmaceuticals

摘　　要：目的优化红荷山葡降脂胶囊的制备工艺,并建立测定方中君药红曲的指标性成分洛伐他汀含量的高效液相色谱法。方法采用单因素试验,以休止角、吸湿性、堆密度、样品颜色等为考察指标,筛选最佳辅料、配比及混合时间,并确定胶囊型号及装量。色谱柱为Thermo Hypersil GOLD C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(75∶25,V/V)等度洗脱,流速为1.0 mL/min,检测波长为237 nm,柱温为30℃,进样量为10μL。结果最优制备工艺条件为原料粉(红曲粉+荷叶-山楂共煎提取物+葡萄籽提取物)-药用糊精-二氧化硅(44∶1∶3,m/m/m),混合20 min;3批小试样品中洛伐他汀含量的平均值为22.31 mg/g。堆密度为0.46 g/mL,空心胶囊选择0号胶囊,装量规格为每粒0.34 g。洛伐他汀溶液质量浓度在9~90μg/mL范围内与峰面积线性关系良好(R2=1,n=8);精密度、稳定性、重复性、加样回收试验的RSD均小于3.0%。结论优化的制备工艺操作简便,工艺合理可行,可为大生产提供科学依据。所建立的含量测定方法操作简便,结果准确,稳定性和重复性均较好,可用于红荷山葡降脂胶囊的质量控制。Objective To optimize the preparation process of Hongheshanpu Lipid-Lowering Capsules,and to establish a high-performance liquid chromatography(HPLC)method for the content determination of lovastatin,an index component of Monascus.Methods Single factor test was used to screen the best excipient,ratio and mixing time,and determine the model and loading capacity of the capsule with angle of recluse,hygroscopicity,pile density and sample color as the inspection indexes.The chromatographic column was Thermo Hypersil GOLD C18 column(250 mm×4.6 mm,5μm),the mobile phase was methanol-water(75∶25,V/V)with isocratic elution,the flow rate was 1.0 mL/min,t he detection wavelength was 237 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The optimum preparation conditions were as follows:raw material powder(Monascus powder+Nelumbinis Folium-Hawthorn co-decocted extract+Vitis Fructus extract)-medicinal dextrin silica(44∶1∶3,m/m/m),mixed for 20 min.The average content of lovastatin in three batches of small test samples was 22.31 mg/g.The bulk density was 0.46 g/mL.Capsule No.0 was canned,and the loading specification was 0.34 g per capsule.The mass concentration of lovastatin solution showed a good linear relationship with the peak area in the range of 9-90μg/mL(R2=1,n=8).The RSDs of precision,stability,repeatability and recovery tests were less than 3.0%.Conclusion The optimized preparation process is simple,reasonable and feasible,and can provide a scientific basis for large-scale production.The established method for content determination is simple,accurate,stable and reproducible,which can be used for the quality control of Hongheshanpu Lipid-Lowering Capsules.

关 键 词：红荷山葡降脂胶囊 洛伐他汀 制备工艺 含量测定 高效液相色谱法 

分 类 号：R932[医药卫生—生药学] R286.0[医药卫生—药学]