摘要
目的:建立红外光谱液体池法分析测定卤化丁基橡胶塞表面残留硅油含量,并对其影响因素进行了评价。方法:样品经四氯化碳溶剂回流提取,溶剂蒸干后,用甲苯溶解定容,直接加样至0.5 mm KBr液体池,在(1260±10)cm^(-1)特征峰进行红外光谱定量扫描测定。结果:二甲硅油的标准系列溶液在0.2~5.0 mg/mL浓度范围内,具有良好的线性关系,回归方程为A=0.2596C+0.0029,r=0.9999。按低、中、高浓度水平加标,回收率为94.8%~98.0%。结论:建立的红外光谱液体池法具有较高的专属性,操作简便等优点,可适用于不同规格不同配方的卤化丁基橡胶塞表面残余硅油的分析检测。
Objective:To establish a method for analysis of residual polydimethylsiloxane on the surface of halogenated butyl rubber stoppers followed by infrared liquid pool spectrometry.Methods:The halogenated butyl rubber stoppers were extracted by carbon tetrachloride(CCl4)through reflow.After vaporizing CCl4 absolutely,the extraction was dissolved and diluted into definite amount of toluene.Then the final mixture was directly loaded into 0.5 mm KBr liquid pool for the infrared spectrometry screening at(1260±10)cm-1.Results:The series concentration of polydimethylsiloxane standard exhibited good linearity ranging from 0.2 mg/mL to 5.0 mg/mL,and the obtained regression equation A=0.2596C+0.0029 represented the correlation coefficient factor 0.9999.The recoveries ranged from 94.8%to 98.0%when spiked with low,medium and high concentration of control standards respectively.Conclusions:The developed method has the advantages of high specificity,simple operation and exhibits great application potential in the analysis and determination of residual polydimethylsiloxane on the surface of halogenated butyl rubber stoppers with different specifications and formulations.
作者
颜萍
何开勇
江燕
胡敏
YAN Ping;HE Kaiyong;JIANG Yan;HU Min(Hubei Institute for Drug Control,Hubei Engineering Research Center for Drug Quality Control,Wuhan Hubei 430075,China.)
出处
《药品评价》
CAS
2022年第22期1353-1356,共4页
Drug Evaluation
关键词
药物残留物
卤化丁基橡胶塞
硅油
谱学
近红外线
Drug residues
Halogenated butyl rubber stoppers
Polydimethylsiloxane
Spectroscopy,near-Infrared
