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目的:建立傅立叶变换衰减全反射红外光谱(FTIR-ATR)法测定药用卤化丁基橡胶塞表面硅油量。方法:样品经乙醚回流提取,溶剂挥干后,用三氯甲烷溶解并定容,直接加样至傅立叶变换红外光谱仪的ZnSe晶体样品槽,扫描红外谱图。利用二甲基硅油在(1260±10)cm-1波数的特征吸收峰峰面积定量测定。结果:二甲基硅油在1.2～32.1 mg·mL-1范围内呈良好的线性关系,r=0.9983。二甲基硅油的LOQ为1.2 mg·mL-1,平均回收率为92.1%。结论:本方法灵敏,准确可靠,可用于药用卤化丁基橡胶塞表面残留硅油的定量测定。
Objective: To establish a Fourier transform attenuated total reflection infrared spectroscopy (FTIR-ATR) method for the determination of silicone oil on the surface of medicinal halogenated butyl rubber plugs. Methods: The sample was extracted by diethyl ether. The solvent was evaporated to dryness and then dissolved in chloroform. The sample was directly loaded into the ZnSe crystal sample cell of Fourier transform infrared spectrometer to scan the infrared spectrum. The peak area of characteristic absorption peak of (1260 ± 10) cm-1 was quantitatively determined with dimethicone. Results: Dimethicone had a good linearity in the range of 1.2 ~ 32.1 mg · mL-1, r = 0.9983. The LOQ of simethicone was 1.2 mg · mL-1 and the average recovery was 92.1%. Conclusion: The method is sensitive, accurate and reliable and can be used for the quantitative determination of residual silicone oil on the surface of medicinal halobutyl plug.