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溶胶-凝胶-硫化法制备硅橡胶吸附萃取搅拌棒的机理及其应用
Mechanism for Preparation of Silicon Rubber Sorptive Extraction Stir Bar by Sol-Gel-Sulfuration Method and Its Application
  
DOI：
中文关键词: 硅橡胶；溶胶-凝胶-硫化法；吸附萃取；搅拌棒；涂层；气相色谱分析
英文关键词: silicone rubber；sol-gel-sulfurization method；sorptive extraction；stir bar；coating；gas chromatography analysis
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中图分类号:TQ333.93；TQ336.4
Author NameAffiliation
JI Xiangjuan Lunan Institute of Coal and Chemical Industry Research 
LIU Tao Lunan Institute of Coal and Chemical Industry Research 
XU Ruiping Lunan Institute of Coal and Chemical Industry Research 
WANG Li Lunan Institute of Coal and Chemical Industry Research 
YIN Huijun Lunan Institute of Coal and Chemical Industry Research 
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中文摘要:
      搅拌棒吸附萃取技术是一种绿色环保、高效富集的新型样品预处理技术。以甲基乙烯基硅橡胶、乙烯基封端硅橡胶和甲基硅橡胶为主体材料，采用溶胶-凝胶-硫化方式成型吸附萃取搅拌棒涂层。结果表明：硅烷偶联剂KH-560加入方式、硫化方式和老化方式对搅拌棒硅橡胶涂层成型影响较大，采用硅烷偶联剂KH-560先水解再加入胶液、分阶段硫化和多阶段升温老化法成型的搅拌棒涂层表面形貌规则，平均厚度为150～250 μm，萃取体积约为25 μL，热分解温度为300 ℃；对搅拌棒富集的胸腺五肽中残留的有机溶剂进行气相色谱分析，取得较好效果；搅拌棒使用寿命可达150次。
英文摘要:
      As a new sample pre-treatment technology，stir bar sorptive extraction has high efficient enrichment and is environmentally-friendly.In this study，the sorptive extraction coating on stir bar was formed by the sol-gel process and sulfurization treatment，using methyl vinyl silicone rubber，vinyl terminated silicone rubber and methyl silicone rubber as the main materials.It was found that，the adding method of silane coupling agent KH-560，curing method and the aging method had significant influence on the formation of a silicone rubber coating.When silane coupling agent KH-560 was hydrolyzed first and then added into the coating mixture，and multiple stage curing and multi-stage high temperature aging were applied，the coating morphology was uniform，the average coating thickness was 150～250 μm，the extraction volume was approximately 25 μL and the decomposition temperature reached 300 ℃.The stir bar was tested in sorptive extraction of thymic pentapeptide and the gas chromatography analysis results of the residual organic solvents enriched by the stir bar showed good results.The stir bar could be re-used up to 150 times.
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