Determination of N,N-Dimethylaniline in Quetiapine Fumarate by LC-MS / 医药导报

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.