丁基羟基苯甲醚有关物质测定的方法研究  

Determination of the related substances in butylated hydroxyanisole

作　　者：伍伟聪[1] 陈英[1] 王淼[1] 王彩媚[1] WU Weicong;CHEN Ying;WANG Miao;WANG Caimei(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《中国药品标准》2021年第4期309-314,共6页Drug Standards of China

基　　金：《中国药典》2015年版药用辅料增修订研究课题(课题编号:76);广东省仿制药质量和疗效一致性评价研究平台(广东省科技厅项目,2017B020221002)。

摘　　要：目的:建立丁基羟基苯甲醚的有关物质测定方法。方法:HPLC法,采用十八烷基硅烷键合硅胶(4.6 mm×250 mm,5μm)色谱柱,以冰醋酸溶液(5→100)-乙腈(40∶60)为流动相;流速:1.0 mL·min^(-1);检测波长:275 nm。结果:丁基羟基苯甲醚与各杂质峰均能良好分离,3-叔丁基-4-羟基苯甲醚在0.5~10μg·mL^(-1)(r=0.9999,n=5)、对苯二酚在0.5~10μg·mL^(-1)(r=0.9999,n=5)范围内线性关系良好,对苯二酚对3-叔丁基-4-羟基苯甲醚的相对校正因子为0.753。3-叔丁基-4-羟基苯甲醚的定量限与检测限分别为0.05和0.04μg·mL^(-1)。14批丁基羟基苯甲醚样品测定结果显示,最大杂质含量均小于0.1%,杂质总量均小于0.3%。结论:经方法学验证,本方法灵敏、专属性强,准确性高,各成分分离度良好,可用于丁基羟基苯甲醚有关物质的测定。Objective:To establish a method for determination of the related substances in butylated hydroxyanisole.Methods:The test was performed in octadecylsilane bonded silica gel column(4.6 mm×250 mm,5μm)under the isocratic elution of glacial acetic acid solution(5→100)and acetonitrile(40∶60).The flow rate was 1.0 mL·min^(-1) and the detection wavelength was 275 nm.Results:The peaks of butylated hydroxyanisole and impurity peaks were separated well.The linear ranges of 3-tert-butyl-4-hydroxyanisole and hydroquinone fell into 0.5-10μg·mL^(-1)(r=0.9999,n=5)and 0.5-10μg·mL^(-1)(r=0.9999,n=5),respectively.The relative correction factor of hydroquinone to 3-tert-butyl-4-hydroxyanisole was 0.753.The LOQ and LOD of 3-tert-butyl-4-hydroxyanisole were 0.05μg·mL^(-1) and 0.04μg·mL^(-1),respectively.The test results of 14 batches of butylated hydroxyanisole samples showed that the content of maximum impurity was less than 0.1%and the content of total impurities was less than 0.3%.Conclusion:The method validation results show that the established method was sensitive,specific and accurate,and has the good resolutions.It can be used for determination of the related substances in butylated hydroxyanisole.

关 键 词：丁基羟基苯甲醚 对苯二酚 有关物质 高效液相色谱法 

分 类 号：R921.2[医药卫生—药学]