摘要
目的建立同时测定甲苯磺酸拉帕替尼原料药中残留溶剂1，2．二甲氧基乙烷、四氢呋喃、甲醇、二氯甲烷、甲苯、乙酸乙酯、异丙醇残留量的方法。方法采用顶空进样气相色谱法，以N，N-二甲基乙酰胺为溶剂，外标法计算残留溶剂量。色谱柱为DB．624，起始温度为45℃，维持3min，再以每分钟20＊C的速率升温至230℃，维持3mira进样口温度为200℃；检测器温度为280℃；顶空瓶平衡温度为80℃；平衡时间为20min；载气为氮气，流速为2．0mL／min。结果7种残留溶剂在考察的浓度范围内线性关系良好（r=0．9980～0．9998）；平均加样回收率为96．57％～100．79Vo（RSD=0．95％-3．21％）。结论该方法操作简单、方法灵敏、结果准确，可用于甲苯磺酸拉帕替尼原料中残留溶剂检查。
Objective To develop a method for the determination of 7 residual organic solvents（1,2- Dimethoxyethane, tetrahydrofuran, methanol, dichlormethane, methylbenzene, ethyl acetate, isopropanol）in lapatinib ditosylate. Methods Headspace GC method was adopted. The determination was performed on a agilent DB-624 capillary column with FID detector. The solvent was dimethylformamide. The injector temperature was set at 200 ℃ and the detector temperature was 280 ℃ by temperature programming. The flow rate was 2 mL/min with headspace and temperature programmed. Results The good linear relation of 7 kind of organic solvents were achieved（r=0.9980-0.9998）. The average recoveries ranged from 96.57% to 100.79%（RSD = 0.95%-3.21%）. Conclusion The method is simple, sensitive and accurate, and can be used for the determination of residual organic solvents in lapatinib ditosylate.
出处
《国外医药（抗生素分册）》
CAS
2016年第2期77-80,共4页
World Notes on Antibiotics
关键词
甲苯磺酸拉帕替尼
原料药
顶空进样气相色谱法
残留溶剂
lapatinib ditosylate： raw material
headspace gas chromatography
residual organic solvents
