气相色谱法测定联苯乙酸原料药中5种有机溶剂残留量

Content Determination of 5 Kinds of Residual Organic Solvents in Felbinac Raw Material by GC

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.