摘要
Abstract
Objective To establish a GC-MS method for the determination of the genotoxic impurity ethyl methanesulfonate in starting material of Pemetrexed Disodium by GC-MS. Methods GC-MS was conducted,and the samples were dissolved by N,N-Dimethylfor-mamide. The column was Agilent DB-624(30 mm × 0. 32 mm,1. 8 μm) capillary column,the inlet temperature was 150 ℃,column flow was 3. 0 mL/min(linear velocity was 65 cm/s),carrier gas was high purity helium,column temperature was set at 120 ℃,hold for 2 min,then increased to 165 ℃ at 15 ℃ /min,split injection,split ratio was 10 :1,the detector is a mass spectrometer detector with a electron impact ion source,ion source temperature was 230 ℃,scanning(detection)method was selective ion monitoring,detector voltage was 0 kV(respect to the tuning results),the interface temperature was 200 ℃,the delay time of solvent was 2. 5 min,the injec-tion volume was 2 μL,the concentration was calculated by standard curve. Results The specificity of the method was good,the LOD and LOQ were 0. 11 μg/g(S/ N=3)and 0. 38 μg/g (S/ N=10)in starting material. The calibration curve was linear in the range of 7. 99-159. 84 ng/mL,the recoveries were 97. 94%(n=9),RSD was 3. 85%(n=6). RSD of precision was 8. 52%(n=6),and RSD of repeatability was 1. 09%(n=6). Conclusion The method has good specificity and high accuracy,which can be used to measure the genotoxic impurity ethyl methanesulfonate in starting material of Pemetrexed Disodium.关键词
气相色谱-质谱联用法/培美曲塞二钠起始原料/遗传毒性杂质/甲磺酸乙酯Key words
GC-MS/Pemetrexed Disodium starting material/genotoxic impurity/ethyl methanesulfonate分类
医药卫生
