HPLC法检查奥拉帕利原料中有关物质
HPLC determination of related substances in olaparib raw materials
邹艳 1吴海龙 1邓丽 1胡川 2李宏名1
作者信息
- 1. 国药集团川抗制药有限公司,成都 611731
- 2. 成都康弘药业集团股份有限公司,成都 610000
- 折叠
摘要
目的:建立高效液相色谱法检测奥拉帕利原料中的有关物质.方法:采用YMC-Pack pro C18 AS(150 mm×4.6 mm,3 μm)色谱柱,以0.05 mol·L-1的磷酸二氢钾(用稀磷酸调pH至3.0)-甲醇-乙腈(90∶5∶5)为流动相A,甲醇-乙腈-水(45∶45∶10)为流动相B,进行梯度洗脱,流速0.8 mL·min-1,柱温30℃,检测波长210 nm,进样量10 μL.结果:空白溶剂不干扰供试品溶液有关物质测定,系统适用性溶液中已知杂质Ⅰ～Ⅶ及未知杂质在该色谱系统中分离完好;奥拉帕利质量浓度在0.033～411.623 μg·mL-1,杂质Ⅰ～Ⅶ质量浓度均在0.05～3.0 μg·mL-1与其峰面积呈较好的线性关系,其r均在0.999以上;杂质Ⅰ～Ⅶ平均回收率均大于92.0％(RSD均小于4.0％).结论:HPLC法检查奥拉帕利原料有关物质方法专属性强,灵敏度高,准确度高,精密度好,可满足奥拉帕利原料有关物质检测需求.
Abstract
Objective:To establish an HPLC method for the determination of related substances in olaparib raw materials.Methods:By using YMC-Pack pro C18 AS(150 mm × 4.6 mm,3 μm)column,0.05 mol·L-1 potassium dihydrogen phosphate(pH 3.0 adjusted with dilute phosphoric acid)-methanol-acetonitrile(90∶5∶5)was as mobile phase A and methanol-acetonitrile-water(45∶45∶10)was as mobile phase B,in gradient elution,with flow rate of 0.8 mL·min-1.The column temperature was 30 ℃,the detection wavelength was 210 nm,and the injection volume was 10 μL.Results:The solvent blank did not interfere with the determi-nation of relevant substances in the test solution,the known impurities Ⅰ-Ⅶ and unknown impurities in the system suitability solution were well separated in the chromatographic system.Olaparib had a good linear relationship with its peak area in the concentration range of 0.083-333.133 μg·mL-1.The concentrations of impurities Ⅰ-Ⅶ were 0.05-3.0 pg·mL-1,there were good linear relationships with their peak area,and their r were 0.999 7 or above.The average recoveries of impurities Ⅰ-Ⅶ were all above 92.0％,and RSDs were less than 4.0％.Conclusion:The HPLC method for the detection of the related substances of olaparib raw materials has strong specificity,high sensitivity,high accuracy and good precision,which can meet the require-ments for the detection of related substances of olaparib raw materials.
关键词
奥拉帕利/聚腺苷二磷酸核糖聚合酶(PARP)抑制剂/有关物质/方法研究/质量控制/高效液相色谱Key words
olaparib/PARP inhibitor/related substances/method study/quality control/high performance liquid chromatography(HPLC)引用本文复制引用
出版年
2024
NETL
NSTL
万方数据