医药导报2017，Vol.36Issue(3)：317-320,4.DOI:10.3870/j.issn.1004-0781.2017.03.018
液相色谱-质谱联用测定富马酸喹硫平中N,N-二甲基苯胺
Determination of N,N-Dimethylaniline in Quetiapine Fumarate by LC-MS
梁键谋 1傅聪 2陈悦1
作者信息
- 1. 浙江省食品药品检验研究院化学药品检验所,杭州310052
- 2. 浙江医药高等专科学校,宁波317503
- 折叠
摘要
Abstract
Objective To establish a LC-MS analytical method for determination of N,N-dimethylaniline which is genotoxic impurity in quetiapine fumarate.Methods The method was achieved by an Waters ACQUITY UPLC CSHTM PhenylHexyl(2.1 mm× 100 mm,1.7 μm) utilizing a mobile phase of buffer-methanol(900∶ 100) (A)-acetonitrile(B) with gradient elution at the flow rate of 0.4 mL·min-1.The temperature of column was set at 50 ℃;The DIONEX Ultimate 3000 HPLC-AB Science 4000 QTrap Tripling Four bar LC-MS to detect N,N-Dimethylaniline (ESI source,in MRM positive mode).Results Standard curve was linear in the range of 0.4-8.0 ng(r =0.999 3);The limit of detection was 0.2 ng;The limit of quantification of N,N-dimethylaniline was 0.4 ng,respectively.The average recovery of N,N-dimethylaniline was 103.3 ％;RSD was 4.3％ (n =9),respectively.Conclusion The method is convenient and sensitive for the determination of N,N-dimethylaniline in quetiapine fumarate.关键词
喹硫平,富马酸/N,N-二甲基苯胺/基因毒性/液质联用Key words
Quetiapine, fumarate/N, N-dimethylaniline/Genotoxic impurities/Liquid chromatography-mass spectrometry分类
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梁键谋,傅聪,陈悦..液相色谱-质谱联用测定富马酸喹硫平中N,N-二甲基苯胺[J].医药导报,2017,36(3):317-320,4.
