布洛芬原料及制剂有关物质的研究  

Related Substances study in Ibuprofen Raw Materials and Its Preparations

作　　者：张秉华 王发 孟新芳 徐长根 刘海静 丁丽霞[2] 杜冠华[3] 

机构地区：[1]陕西省食品药品检验所,西安710061 [2]中国药学会,北京100022 [3]中国医学科学院-北京协和医学院药物研究所,北京市药物靶点研究与新药筛选重点实验室,北京100050

出　　处：《中国药学杂志》2013年第8期640-643,共4页Chinese Pharmaceutical Journal

基　　金：卫生部公益性行业科研专项(200902008)

摘　　要：目的建立布洛芬原料、片剂和胶囊中有关物质的分析方法。方法采用高效液相色谱法测定已知杂质2-(4-异丁基苯基)丙酸、4-异丁基苯甲酸、羟苯甲酯钠(中检院提供杂质);4'-异丁基苯乙酮(日本药局方已知杂质);已知杂质A、J、N(欧洲药典已知杂质)以及布洛芬中的未知杂质。色谱柱:Kromasil C18(4.6 mm×250 mm,5μm);流动相:乙腈-水(磷酸调节pH为3.0)(45∶55);流速:1.0 mL.min-1;检测波长:254 nm;柱温:35℃。结果布洛芬原料、片剂、胶囊中的已知杂质主要为4-异丁基苯甲酸和4'-异丁基苯乙酮,同时发现国内个别厂家制剂中的未知杂质也较高。结论新制定的高效液相色谱方法能够很好的对布洛芬原料及制剂的有关物质进行控制,可同时测定。OBJECTIVE To establish the determination method of the related substances in ibuprofen raw materials, tablets and capsules. METHODS High performance liquid chromatography （HPLC） was used for the determination of 2-（ 4-isobutyl phenyl ） propanoic acid, 4-isobutyl benzoic acid, sodium methyl hydroxybenzoate（provided by national institutes for food and drug control） , 4＇- isobutyl acetophenone（known impurities of JP）, the relative substance A, J, N（known impurities of EP） , and the unknown impurities. A Kromasil Cts column （4.6 mm × 250 mm, 5 μm） was used as the analytical column, acetonitrile-water （ pH adjusted to 3.0 by phosphoric acid） （45： 55） were used as the mobile phase, the flowing rate was 1.0 mL . min^-1, the detection wavelength was set at 254 nm, and the column temperature was 35 ℃. RESULTS The relative substances detected in ibuprofen raw materials and its preparations were mainly 4-isobutyl benzoic acid and 4＇-isobutyl acetophenone. The contents of unknown impurities were also high in the preparations of some manufacturers. CONCLUSION The method can be used for the analysis of the related substances in ibuprofen raw materials and its preparations.

关 键 词：布洛芬原料 布洛芬制剂 高效液相色谱法 有关物质 2-(4-异丁基苯基)丙酸 4-异丁基苯甲酸 

分 类 号：R917[医药卫生—药物分析学]