CAJ | 학술논문

目的：：建立甲磺酸伊马替尼中4-甲基-N-[4-(3-吡啶基)-2-嘧啶基]苯-1,3-二胺的测定方法。方法：采用LC-MS/MS法测定；ESI离子源,正离子模式；用MRM方式进行扫描,选择离子对为278.1/106.1；以甲酸铵溶液-甲酸的乙腈溶液进行梯度洗脱。结果：本成分在1.572~47.160 ng·ml-1范围内线性关系良好(r =0.9997),检出限为0.0021 ng,定量限为0.0068 ng,平均回收率为100.9%(RSD=2.88%),专属性、溶液稳定性、重复性、耐用性等试验结果均符合规定。结论：该法可用于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,明显优于已见报道的其他文献方法。
목적：：건립갑광산이마체니중4-갑기-N-[4-(3-필정기)-2-밀정기]분-1,3-이알적측정방법。방법：채용LC-MS/MS법측정；ESI리자원,정리자모식；용MRM방식진행소묘,선택리자대위278.1/106.1；이갑산안용액-갑산적을정용액진행제도세탈。결과：본성분재1.572~47.160 ng·ml-1범위내선성관계량호(r =0.9997),검출한위0.0021 ng,정량한위0.0068 ng,평균회수솔위100.9%(RSD=2.88%),전속성、용액은정성、중복성、내용성등시험결과균부합규정。결론：해법가용우측정갑광산이마체니중4-갑기-N-[4-(3-필정기)-2-밀정기]분-1,3-이알,명현우우이견보도적기타문헌방법。
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.