高效液相梯度洗脱法测定阿托伐他汀钙片有关物质  

Determination of Related Substances in Atorvastatin Calcium Tablets by HPLC Gradient Elution

作　　者：熊苗苗[1] 汪秋兰[1] 谢斌 王文清[1] 方建国[1] 

机构地区：[1]华中科技大学同济医学院附属同济医院药学部,武汉430030 [2]湖北丝宝药业有限公司,武汉430019

出　　处：《医药导报》2013年第5期656-660,共5页Herald of Medicine

摘　　要：目的建立测定阿托伐他汀钙片有关物质的高效液相色谱法。方法采用梯度洗脱方法,色谱柱为Apollo C18(4.6 mm×250 mm,5μm),以流动相A醋酸铵缓冲液[称取醋酸铵1.54 g,置1 000 mL水中,用冰醋酸调节pH至(4.50±0.05)]-乙腈(70∶30),流动相B乙腈进行梯度洗脱,流速:1.1 mL·min-1,检测波长:244 nm,柱温:40℃,进样量:20μL。对照杂质对照品对照法和不加校正因子的主成分自身对照法检查。结果阿托伐他汀主峰与各杂质峰均能良好分离。杂质A、B、C、D、H和I分别在0.190 4～9.519 8,0.203 2～10.160 0,0.191 2～9.560 0,0.208 0～10.400 0,0.198 8～9.940 0,0.205 2～10.260 0μg.mL-1范围内具有良好的线性关系。平均回收率分别为100.24%,99.73%,94.47%,92.17%,103.76%,101.23%。结论该方法快速,结果准确可靠,可用于阿托伐他汀钙片的有关物质检查。Objective To establish a method for determination of related substances in atorvastatin calcium tablets by high performance liquid chromatography （HPLC）. Methods The gradient elution was used with the column Apollo C^8 （4.6 mm×250mm,5μm）. Ammonium acetate buffer solution （1.54 g ammonium acetate dissolved in 1 000 mL water and adjusted to pH 4.50~0.05 with acetic acid）-acetonitrile （70 ： 30） and aeetonitrile was served as the mobile phase A and B, respectively. The flow rate was 1.1 mL·min^-1 , detective wavelength was 244 nm, column temperature was at 40 ℃ , and sample was load as 20μL. Determination with reference substance and main component self-comparison without calibration factor were performed. Results Atorvastatin was isolated from the impurities successfully. Impurity A, B, C, D, H and I had a good linearity in the range of 0. 190 4-9. 519 8, 0. 203 2- 10. 160 0,0. 191 2-9. 560 0,0. 208 0- 10. 400 0,0. 198 8- 9. 940 0μg·mL^-1 ,and 0. 205 2-10. 260 0μg·mL^-1 , respectively. And the average recoveries were 100.24% , 99.73% , 94.47%, 92.17%, 103.76% and 101.23%. Conclusion This method is proved to be rapid, accurate and reliable. It is suitable for determination of related substances in atorvastatin calcium tablets.

关 键 词：阿托伐他汀钙 有关物质 色谱法 高效液相 梯度洗脱 

分 类 号：R972.6[医药卫生—药品] R927.1[医药卫生—药学]