FTIR-ATR法测定药用卤化丁基橡胶塞表面二甲基硅油残留量和在葡萄糖氯化钠注射液中的迁移量

目的：建立傅立叶变换衰减全反射红外光谱法（FTIR-ATR法）测定药用卤化丁基橡胶塞表面的二甲基硅油残留量，并对其在葡萄糖氯化钠注射液中的迁移进行研究。方法：橡胶塞样品以及葡萄糖氯化钠注射液分别经二氯甲烷振荡提取、萃取，挥干溶剂，用定量的三氯甲烷溶解，采用衰减全反射法（ATR法），直接加样至傅立叶变换红外光谱仪的金刚石晶体表面，立即扫描红外光谱图，测定定量峰面积，以回归方程计算，即得橡胶塞表面二甲基硅油残留量以及其在葡萄糖氯化钠注射液中的迁移量。结果：在测定橡胶塞表面二甲基硅油残留量的试验中，二甲基硅油质量浓度在1.2~50.0 mg·mL^-1范围内呈良好的线性关系（R²=0.998 9），二甲基硅油的定量下限为1.2 mg·mL^-1，平均回收率（n=9）为99.1%，测得橡胶塞表面二甲基硅油残留量在0~25.9 μg·cm^-2；在葡萄糖氯化钠注射液中二甲基硅油的迁移研究试验中，塞有橡胶塞的注射剂瓶倒置第5天、第10天和第20天，注射液中二甲基硅油迁移量分别为144.6、157.7、185.7 μg，迁移率分别为3.15%、3.43%、4.04%，而正置注射剂瓶中的二甲基硅油迁移量均为0。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二甲基硅油的定量测定；实验表明药用橡胶塞表面残留二甲基硅油会向葡萄糖氯化钠注射液中迁移，其迁移量随着时间的增加而增加。

Objective:To establish a Fourier transform infrared spectroscopy-attenuated total reflection spectra (FTIR-ATR) method for determination of residual polydimethylsiloxane on the surface of medical halogenated butyl rubber stopper, and also to study its migration in the glucose and sodium chloride injection.Methods:Oscillating extract the rubber stopper samples and glucose and sodium chloride injectionusing dichloromethane, respectively;dry the solvent, dissolve the dryness with a quantitative trichloromethane and mix well.Transfer the mixture directly to the diamond crystal surface of Fourier transform infrared spectrometer, and then scann the infrared spectrum immediately by the attenuated total reflection (ATR) method, determine quantitative peak area and calculate the content of polydimethylsiloxane by regression equation.The residual amount of polydimethylsiloxane on the surface of rubber stopper and its migration amount in glucose and sodium chloride injection was obtained.Results:The linear range of polydimethylsiloxane was 1.2-50.0 mg·mL^-1 with the correlation coefficient of 0.998 9, the LOQ of polydimethylsiloxane was 1.2 mg·mL^-1, the average recovery of the method (n=9) was 99.1%.The residual amount of polydimethylsiloxanel on the surface of rubber stopper samples was 0-25.9 μg·cm^-2.The migration amounts of the injection bottles with rubber stopper inverted position were 144.6 μg, 157.7 μg and 185.7 μg respectively in the fifth, tenth and twentieth days, and the migration rates were 3.15%, 3.43% and 4.04% respectively, while the migration amounts of the positive injection bottles were 0.Conclusion:This method is sensitive, accurate and reliable, it can be used for quantitative determination of polydimethylsiloxane on the surface of medical rubber stopper, the experiments showed that the residual polydimethylsiloxane on the surface of the medical rubber stopper will migrate to glucose and sodium chloride injection, and the migration amount increased with time.

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