Determination of 4-Methyl-N-(4-(pyridin-3-yl) pyrimidin-2-yl) benzene-1, 3-diamine in Imatinib Mesylate by LC-MS/MS
- VernacularTitle:LC-MS/MS法测定甲磺酸伊马替尼中4-甲基-N-[4-（3-吡啶基）-2-嘧啶基]苯-1,3-二胺
- Author:
Shuhua WANG
;
Panhai LI
;
Hengchang ZANG
;
Haixia YANG
;
Xiuzhen WANG
- Publication Type:Journal Article
- Keywords:
Imatinib mesylate;
Impurity;
LC-MS/MS;
Determination
- From:
China Pharmacist
2014;(12):2030-2032
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To establish a method for the determination of 4-methyl-N-(4-(pyridin-3-yl) pyrimidin-2-yl) benzene-1,3-diamine as an impurity in the preparation of imatinib mesylate. Methods: An LC-MS/MS method was used with ESI ion source con-trolled by a positive-ion mode. The MRM mode was performed with 278. 1/106. 1 as the scanning and ion-pair. Acetonitrile solution containing ammonium formate and formic acid was used with gradient elution. Results:The linear range was 1. 572~47. 160 ng/ml(r=0. 999 7). The detection limit was 0. 002 1ng and the limit of quantitation was 0. 006 8ng. The average recovery was 100. 9% with RSD of 2. 88. The results of specificity, solution stability, repeatability and durability all met the specification. Conclusion:The meth-od is sensitive, accurate and special in the determination of 4-methyl-N-(4-(pyridin-3-yl) pyrimidin-2-yl) benzene-1,3-diamine in imatinib mesylate.
