Determination of Erlotinib Hydrochloride by Proton Nuclear Magnetic Resonance
10.3870/j.issn.1004-0781.2017.12.017
- VernacularTitle:1H-核磁共振定量法测定盐酸厄洛替尼含量
- Author:
Chengxin LI
1
;
Xueping WANG
;
Feng CUI
;
Haijun HAO
Author Information
1. 中国医药工业研究总院上海医药工业研究院分析测试中心
- Keywords:
Erlotinib;
hydrochloride;
Nuclear magnetic resonance;
Quantitative analysis
- From:
Herald of Medicine
2017;36(12):1398-1401
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a rapid and accurate method for quantitative determination of erlotinib hydrochloride by proton nuclear magnetic resonance(1H-NMR). Methods Maleic acid was used as an internal standard,and DMSO-d6 was employed as solvent.The pulse width was 9.54 μs,the delay time was 20 s,the scanning frequency was 64 and the testing temperature was set as 300℃.Under this condition,the 1H-NMR data of the mixture of erlotinib hydrochloride and maleic acid were obtained.The content of erlotinib hydrochloride was calculated by comparing the response signal area of sample (As) and internal standard (Ar). Results Proton signal peaked at δ 8.84 and δ 8.47 for erlotinib hydrochloride and at δ6.26 for maleic acid served as quantitation peaks.The content of erlotinib hydrochloride was obtained by calculating the average of the test results of the two quantitative peaks.The concentration of erlotinib hydrochloride (2.88~19.08 mg·mL-1) and the peak area of quantification peaks showed a good linear correlation.The precision RSD was 0.36% (n=6),the repeatability RSD was 0.83%(n=6) and the sample recovery was 100.91% (n=6).The content of 3 batches of erlotinib hydrochloride was 92.26%,91.94%and 92.09%,the average was 92.10% and its RSD was 0.17%.The obtained results were generally consistent with those obtained from mass balance method. Conclusion This established method is simple to handle as compared to traditional methods,and the analysis results are accurate.1H-NMR provides a novel method for the determination of erlotinib hydrochloride and can be used for the quality control of erlotinib hydrochloride.
