摘要
目的建立毛细管气相色谱法测定替格瑞洛中7种有机溶剂残留量。方法采用DB-624色谱柱(60 m×0.53 mm,3.0μm),氮气作为载气,采用氢火焰离子化检测器检测,以N,N-二甲基甲酰胺为溶剂,以正己烷为内标物,检测替格瑞洛原料药中残留溶剂。结果二氯甲烷、甲醇、乙酸乙酯、四氢呋喃、正庚烷、乙醇和醋酸线性关系良好(r=0.999 0~0.999 6),平均回收率为99.0%~101.1%,定量限分别为4.23、3.00、2.50、1.44、1.00、2.00和5.01 mg·L^(-1)。结论建立的方法适用于替格瑞洛中7种残留溶剂的同时测定。
Objective To establish a capillary gas chromatography method for the determination of seven kinds of residual solvents in ticagrelor. Methods The samples were separated on DB-624 capillary column （60 m × 0. 53 mm × 3.0 μm ） and analyzed with FID detector. Nitrogen was used as carrier gas and N-hexane was used as the internal standard. Results There were good linear relationships in the experimental concentrations of dichloromethane, methanol, ethyl acetate, tetrahydrofuran, N-heptane, ethanol, acetic acid （r= 0. 999 0-0. 999 6）. The average recoveries were ranged from 99. 0% to 101.1%. The limit of quantification were 3.00,2.00,4. 23,2. 50,1.44,1.00,5.01 mg· L^ -1 , separately. Conclusions The method is simple, sensitive, and accurate with good durability. It can be used for the determination of the seven residual organic solvents in ticagrelor.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2018年第2期125-130,共6页
Journal of Shenyang Pharmaceutical University
关键词
替格瑞洛
溶剂残留
毛细管气相色谱法
内标法
ticagrelor
solvent residue
capillary gas chromatography
internal standard method
