复方甲硝唑克林霉素乳膏的制备及质量控制

摘要

目的 制备复方甲硝唑克林霉素乳膏并建立其质量控制方法.方法 采用乳化法制备乳膏,建立酸碱度、微生物限度、高速离心试验、耐热耐寒试验和室温留样观察试验;采用HPLC、梯度洗脱法,测定乳膏中4种主要成分的含量,色谱柱为Diamonsil C18,流动相:甲硝唑和维生素B4的为乙腈-磷酸氢二钾溶液(0.68％)(20∶80),盐酸克林霉素和螺内酯的为乙腈-磷酸氢二钾溶液(0.68％)(60∶40)流速为1.0 mL/min,检测波长为210 nm,柱温为25℃,进样量为20μL.结果 该乳膏pH为6.0～7.0,微生物限度、高速离心试验、耐热耐寒试验检查等均符合规定.甲硝唑、克林霉素、螺内酯、维生素B6在各自的浓度范围内与峰面积呈良好的线性关系.平均回收率:甲硝唑为100.2％,RSD为0.95％;克林霉素为100.4％,RSD为1.03％;螺内酯为99.60％,RSD为0.99％;维生素B6为99.79％,RSD为0.87％.结论 本品制备工艺简单,所得制剂质量可控,性质稳定,无刺激性,可满足临床需要.含量测定方法简便、快速、结果准确,可用于复方甲硝唑克林霉素乳膏中四种主要成分的含量测定.%Objective To prepare Compound Metronidazole Clindamycin Cream and estabilish a method for its quality control.Methods Compound Metronidazole Clindamycin Cream was prepared by using emulsion process.and then pH,microbial limit,high speed centrifuge test,heat and cold resistant test and room temperature retention test were established.HPLC method for determination of Compound Metronidazole Clindamycin Cream was developed,and gradient elution method was adopted.The chromatography column was Diamonsil C1s;Mobile phase of metronidazole and vitamin B6 was the mixture of acetonitrile and dipotassium hydrogen phosphate (0.68％) (20∶80),and mobile phase of clindamycin hydrochloride and spironolactone was the mixture of acetonitrile and dipotassium hydrogen phosphate (0.68％) (60∶40);the flow rate was 1.0 mL/min;the detection wavelength was 210 nm;the column temperature was 25 ℃,and the sample volume was 20 μL.Results The pH value of the cream was 6.0-7.0,and the quality of cream was eligible in microbial limit,high speed centrifugal test,heat/cold test.Metronidazole,clindamycin,spironolactone and vitamin B6,their respective concentration and peak area showed good linear relationship.The average recovery rates:metronidazole was 100.2％,RSD was 0.95％;clindamycin was 100.4％,RSD was 1.03％;spironolactone was 99.60％,RSD was 0.99％;vitamin B6 was 99.79％,RSD was 0.87％.Conclusion The preparation process is simple,the quality of the preparation is controllable,the property is stable,and the utility model can meet the clinical needs.The method of content determination is also simple,rapid and accurate,can be used for the determination of four main components in Compound Metronidazole Clindamycin Cream.