顶空-气相色谱法测定醋氯芬酸中的残留溶剂

建立了采用顶空-气相色谱法(HS-GC)测定醋氯芬酸中残留溶剂的方法.试验条件:以DB-624(30 m×0.32 mm,1.8μm)为色谱柱,使用氢火焰离子化检测器(FID),柱温为程序升温,顶空平衡温度80℃,平衡时间30 min.结果表明,异丁烯、甲醇、乙酸甲酯和叔丁醇可有效分离,检测限分别为0.013、0.722、0.300和0.550μg/mL.各溶剂线性关系良好,相关系数r均在0.999以上,回收率(n=9)均介于95%~105%之间,RSD均小于10%.方法操作简便,专属性强,准确度高,可应用于醋氯芬酸中残留溶剂的测定.

Determination of Residual Solvents in Aceclofenac by Headspace-Gas Chromatography

A detection method to determine residual solvents in aceclofenac by the headspace-gas chromatography (HS-GC) has been set up. DB-624 (30 m×0.32 mm, 1.8 μm) was used as the chromatographic column, and a hydrogen flame ionization detector (FID) was used in the experiment. The column temperature was programmed, equilibrium temperature and time of headspace were 80 ℃ and 30 min. The results showed that isobutylene, methanol, methyl acetate and tert-butanol can be efficiently separated, and the detection limits were 0.013, 0.722, 0.300, 0.550 μg/mL respectively. For all solvents, the linear relationship was good (r>0.999), the recoveries (n=9) were in the range of 95%~105% and the RSD was less than 10%. The method is of simple operation, strong specificity and high accuracy, and can be used to detect the residual solvents in aceclofenac.