摘要
目的:建立联苯乙酸原料药中5种有机溶剂(甲醇、乙酸乙酯、三氯甲烷、冰醋酸和吗啉)残留量的测定方法。方法:采用气相色谱直接进样法。色谱柱为Agilent DB-624毛管柱,程序升温,载气为氮气,氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。结果:5种溶剂在建立的色谱条件下完全分离,在所考察的线性范围内具有良好的线性关系(r为0.9991~0.9998),平均回收率n97.5%~100.2%,RSD为0.25%~1.39%(n=3)。3批样品中只检出甲醇,且其残留量〈O.3%。结论:建立的方法简便、准确,适用于联苯乙酸原料药中有机溶剂残留量的测定。
OBJECTIVE: To establish the method for the determination of 5 residual organic solvents as/methanol, acetic ether, chloroform, glacial acetic acid and morpholine in felbinac raw material METHODS: Gas chromatography was adopted. The determination was performed on Agilent DB-624 capillary colunm by temperature programming using nitrogen gas as carrier gas. Flame ionization detector was used. The injector temperature was 200 ℃ and the detector temperature was 250 ℃ RESULTS: 5 kinds of solvents were completely separated and determined with a good linearity (r=0.999 1-0.999 8). The average recoveries were 97.5%-100.2%, and RSDs were 0.25%-1.39% (n=3). Only methanol were detected in 3 batches of samples, and residual amount of it was lower than 0.3%. CONCLUSIONS: The method is simple, accurate and suitable for the determination of residual solvents in felbinac raw material.
出处
《中国药房》
CAS
CSCD
2013年第41期3923-3924,共2页
China Pharmacy
关键词
气相色谱法
联苯乙酸原料药
有机溶剂
残留量测定
Gas chromatography
Felbinac raw material
Residual solvent
Residual determination