不同提取方法对氯化丁基胶塞中游离硫测定的影响研究

Study on the influence of different extraction methods on determination of free sulfur in chlorinated butyl rubber stoppers

本文比较了不同提取方法对氯化丁基橡胶塞中硫化剂(游离硫)的提取效果。用4种提取方法对四种氯化丁基橡胶塞进行提取,利用高效液相色谱法对提取液中的游离硫含量进行测定,甲醇-水为流动相,流速1.0 mL/min,检测波长220 nm,紫外检测器。结果表明用4种方法在四种胶塞中均提取出了游离硫。而不同提取方法提取程度有显著区别,其中以使用二氯甲烷-无水乙醇(1∶1)进行回流萃取的方法提取程度最高。研究结果为药用氯化丁基橡胶塞相容性及质量控制提供参考。

This paper compares the effects of different extraction methods on the extraction of vulcanizing agent(free sulfur)from chlorobutyl rubber stoppers.Four extraction methods were used to extract from four batches of chlorinated butyl rubber stoppers,and the free sulfur content in the extracts was determined by high performance liquid chromatography(HPLC)with methanol-water as the mobile phase at a flow rate of 1.0 mL/min and an ultraviolet detector with a detection wavelength of 220 nm.Results showed that free sulfur was extracted from all four batches.The extraction degree of different extraction methods was significantly different,and the reflux extraction method using dichloromethane-anhydrous ethanol(1∶1)was the best.This study provides a reference for the compatibility and quality control of chlorinated butyl rubber stoppers for pharmaceutical applications.