摘要
建立了测定辛伐他汀中抗氧化剂叔丁基羟基茴香醚（BHA）含量的高效液相色谱方法。采用C18色谱柱（Supeleosil C18，4．6mm i．d．×33mm，3μm）；流动相A为乙腈，流动相B为0．1％磷酸水溶液；洗脱梯度为0～3 min 65％B，3～3．5min 65％-45％B，3．5～8．5 min 45％～10％B，8．5-9．5 min 10％B，9．5～10min 10％-65％B，10～11，9 min 65％B，12min stop。检测波长为292 nm，流速为3．0 mL·min^-1，柱温为35℃。结果BHA与辛伐他汀及各杂质分离良好，BHA在0．1～0．9μg·mL^-1范围内峰面积与浓度呈良好的线性关系（r=0．9998），最低检出量为0．4 ng，回收率为99．3％，相对标准偏差为1．0％。该方法简便、快速、准确，可用于辛伐他汀中微量BHA的含量测定。
A method for analysis of butyl hydroxy anisole （BHA, antioxidant） in simvastatin had been establishedby HPLC. Separation and quantification of BHA was carried out on a C18 column （supelcosil C18 column, 4.6mm i.d.×150 mm, 3μm） with a gradient elution of acetonitrile（mobile phase A） and phosphoric acid （0.1%,mobile phase B）. The flow rate was 3.0 ml/min, and BHA was determined with Lrv detector at 292 nm. Gradient： 0-3 min 65 % B,3-3.5 min 65 %-45 % B,3.5-8.5 rain 45 %-10 % B,8.5-9.5 min 10 % B,9.5-10 min 10 % -65 % B,10-11.9 min 65 % B,12 min stop. The experimental results showed a goodseparation of BHA with simvastatin and impurities. Good linear relationship between the peak area and the concentration of BHA was found with correlation coefficient （r） of 0. 9998 within the range of 0.1-0.9 vg/mL.The detection limit of BHA was 0.4 ng and the method recovery was 99.3 % with a relative standard deviationof 1.0 %. The results showed that the method was simple, rapid and accurate for the determination of BHA insimvastatin.
出处
《化工技术与开发》
CAS
2006年第3期17-19,共3页
Technology & Development of Chemical Industry
