电感耦合等离子体发射光谱法测定药用卤化丁基橡胶塞表面硅油量

Determination of Polydimethylsiloxane on the Surface of Pharmaceutical Halogenated Butyl Rubber Stoppers by Inductively Coupled Plasma Optical Emission Spectrometry

目的 建立电感耦合等离子体发射光谱(ICP-OES)法测定药用卤化丁基橡胶塞表面硅油量。方法 样品经航空煤油超声提取后,采用有机相直接进样的方式进行测定。考察发射功率、载气流速、辅助气和等离子体流量,以及样品超声提取时间对硅油含量测定的影响。结果 二甲基硅油在1.0~50μg·mL^(-1)范围内呈良好的线性关系,相关系数(r)为0.999 9。二甲基硅油的定量下限为0.3μg·mL^(-1),加样回收率90.37%~98.34%,相对标准偏差(RSD,n=9)为0.64%~2.22%。结论 该方法灵敏,准确可靠,可用于药用卤化丁基橡胶塞表面硅油的定量测定。

Objective To establish a determination method of polydimethylsiloxane on the surface of halogenated butyl rubber stoppers based on inductively coupled plasma optical emission spectrometry(ICP-OES).Methods The halogenated butyl rubber stoppers were ultrasonic extracted by aviation kerosene.The extraction was determined by direct injection.The effect of different radio frequency power,nebulizer flow,auxiliary gas and plasma flow rate,and ultrasound extraction time on the determination of polydimethylsiloxane were studied.Results The linear range of polydimethylsiloxane was about 1.0-50μg·mL^(-1) and its correlation coefficient was 0.9999.The LOQ of polydimethylsiloxane was 0.3μg·mL^(-1),the average recoveries were 90.37%-98.34%,and the relative standard deviation(RSD,n=9)were 0.64%-2.22%.Conclusion This method is sensitive,accurate,and can be used to determine polydimethylsiloxane on the surface of halogenated butyl rubber stoppers.