摘要
目的：建立盐酸厄洛替尼及其片剂中5种有关物质的定性及定量分析方法。方法：采用高效液相色谱法,使用Waters Symmetry C8色谱柱（4.6 mm×250 mm,5μm）,以0.05 mol·L-1醋酸铵溶液为流动相A,甲醇为流动相B,进行梯度洗脱,流速1.0 m L·min-1,检测波长247 nm,柱温30℃,进样量20μL。分别采用标准曲线法、不加校正因子的主成分自身对照法及加校正因子的主成分自身对照法对有关物质进行定量分析。结果：分别测得了5种杂质对照品的标准曲线及校正因子,杂质A、B、C、D和E的质量浓度分别在0.03~6.10μg·m L-1（r=0.999 7）、0.05~7.62μg·m L-1（r=0.999 8）、0.04~5.80μg·m L-1（r=0.999 8）、0.01~6.00μg·m L-1（r=0.999 7）和0.01~6.41μg·m L-1（r=0.999 9）范围内呈良好的线性关系;各杂质的平均回收率均在98%以上,RSD在2%以下;5种杂质相对于盐酸厄洛替尼的校正因子分别为1.0、1.1、1.1、0.7和0.9。结论：本文采用加校正因子的主成分自身对照法对各已知杂质进行定量,既可以解决杂质对照品提供困难的问题,又可以计算出产品中各杂质的真实含量,可用于盐酸厄洛替尼及其制剂中有关物质的测定。
Objective：To establish a qualitative and quantitative analysis method for the determination of the five related substances in erlotinib hydrochloride and its coated tablets. Methods： The HPLC method was adopted for the analysis. The Waters Symmetry C8 column （4.6 mm × 250 mm,5 μm） was used as the analysis column; the mo- bile phase was 0. 05 tool · L-1 ammonium acetate in water（A） -100% methanol（B） with gradient elution at the flow rate of 1.0 mL · min -1 ; the column temperature was 30 ℃ and the detection wavelength was 247 nm and the injection volume was 20μL. The standard curve method and the main component self-control methods with and without correction factor were used for the quantitative analysis of the related substances respectively. Results： The regression equation and correction factors of five related substances were measured respectively. The results showed that the method had good linearity for impurities A, B, C, D and E in the range of 0. 03-6. 10 μg · mL- 1 （r = 0. 999 7）, 0. 05-7.62 μg· mL - L （ r = 0. 999 8 ）, 0. 04-5.80 μg · mL - 1 （ r = 0. 999 8 ）, 0. 01 - 6. 00 μg · mL - 1 （ r = 0. 999 7 ） and 0. 01-6. 41 μg · mL-1 （r =0. 999 9）. The average recovery of each impurity was more than 98% ,and the average RSD values for precision and reproducibility were both less than 2%. The correction factors of five impurities were 1.0, 1.1,1.1,0. 7 and 0. 9 ,respectively. Conclusion ：The main component self-control method with correction factor in this paper can be used for the qualitative and quantitative analysis of the related substances in erlotinib hydrochlo- ride and its coated tablets ,which not only solve the problem of impurity reference standards＇ availability, but also re-flect the actual contents of each impurity. The method developed in this paper can be used for determination of relat- ed substances in erlotinib hydrochloride and its preparations.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第5期927-933,共7页
Chinese Journal of Pharmaceutical Analysis
