高效液相色谱法测定环孢素胶囊及软胶囊的溶出度  

Determination of the Solubility of Cyclosporine Capsules and Soft Capsules by High Performance Liquid Chromatography

作　　者：庞文哲 韩彬 王强 王茉莉 李香荷 宋更申 PANG Wenzhe;HAN Bin;WANG Qiang;WANG Moli;LI Xianghe;SONG Gengshen(Hebei Institute for Drug Control Institute,Shijiazhuang 050000,China)

机构地区：[1]河北省药品检验研究院,石家庄050000

出　　处：《医药导报》2018年第5期600-604,共5页Herald of Medicine

基　　金：河北省科技厅课题(162776179D)

摘　　要：目的建立测定环孢素胶囊及软胶囊体外溶出度的高效液相色谱法(HPLC)。方法采用篮法测定环孢素胶囊溶出度,以0.1 mol·L^(-1)盐酸(含1.0%十二烷基硫酸钠)1 000 mL为溶出介质,转速为100 r·min^(-1),60 min后取样,采用HPLC法测定。环孢素软胶囊采用桨法,以模拟胃液(胃蛋白酶3.2 g、氯化钠2.0 g、盐酸7.0 mL,N,N-二甲基十二烷基胺-N-氧化物6.9 mL,加水稀释至1 000 mL)为溶出介质,转速75 r·min^(-1),60 min后取样,采用HPLC法测定。色谱条件为:以十八烷基硅烷键合硅胶为填充剂的色谱柱,以四氢呋喃-0.05 mol·L^(-1)磷酸溶液(45∶55)为流动相;柱温为75℃;检测波长220 nm;进样量10μL。结果回归方程为A=10.304C+1.217 5,r=0.999 9;在检测浓度为0.25~9.90μg·mL^(-1)范围内呈良好线性关系。共8个厂家生产的环孢素胶囊及软胶囊溶出度在60 min内均>80%。结论该方法测得的环孢素胶囊及软胶囊的溶出量较高,方法可行性强,灵敏度高,结果准确可靠。Objective To establish a high performance liquid chromatography method for solubility determination of cyclosporin capsules and soft capsules.Methods Solubility of cyclosporine capsules was determined by basket method,with 0.1 mol·L-1 hydrochloric acid solution(1.0%twelve sodium dodecyl sulfate)1 000 mL as dissolution medium at 100 r·min-1.Samples were taken at 60 minute and determined by HPLC method.Paddle method was adopted for the determination of cyclosporin soft capsules with simulate gastric juice(pepsin 3.2 g,sodium chloride 2.0 g,hydrochloric acid 7.0 mL,N,N-two methyl twelve alkyl amine-N-oxide 6.9 mL,dilute with water to 1 000 mL)1 000 mL as dissolution medium at 75 r·min-1,samples were taken at 60 minute and determined by HPLC method.HPLC was performed with C 18 column,The mobile phase consisted of tetrahydrofuran-0.05 mol·L-1 phosphate(45:55).The column temperature was 75℃and the detection wavelength was 220 nm.The injection volume was 10μL.Results The linear range of cyclosporin was 0.25-9.90μg·mL-1(A=10.304 C+1.217 5,r=0.999 9).The accumulative release percentage of the samples from eight manufacturers within 60 min were all above 80%of the stated amount.Conclusion In this condition,dissolution rate of the cyclosporine capsules and soft capsules were high,the method is feasibility and highly sensitive and the result is accurate and reliable.

关 键 词：环孢素胶囊 环孢素软胶囊 溶出度测定 色谱法 高效液相 

分 类 号：R927.11[医药卫生—药学] R979.5