【摘要】 以端羟基聚二甲基硅氧烷为基胶、乙烯基三乙氧基硅烷为封端基团,甲基三甲氧基硅烷为交联剂,在甲基硅油中反应得到封端硫化硅橡胶。将此聚合物涂覆于经氢氧化钾水热处理的镍钛合金纤维丝表面,制得了镍钛合金/硅橡胶固相微萃取头。利用红外光谱法分析了硅橡胶结构,通过热重分析法确定了涂层最高使用温度,扫描甴子显微镜观察了镍钛合金纤维丝和萃取头的表面形貌。通过顶空萃取-固相微萃取-气相色谱(HS-SPME-GC)法测定了西药中丙酮、四氢呋喃、二氯甲烷、乙腈的残留量,各被测物的色谱峰面积与浓度呈良好的线性兲系,线性相兲系数(R2)为0.991 6-0.999 8,最低检测限为0.058-0.235μg/L。实际样品测定的加标回收率为95.9%-99.4%,相对标准偏差为2.35%-3.72%。更多还原

【Abstract】 The terminated vulcanized silicone rubber was prepared by the reaction of hydroxyl-terminated polydimethyl siloxane as base adhesive, vinyl triethoxysilane as sealing group and methyl trimethoxysilane as cross-linking agent in methyl silicone oil. Nickel-titanium alloy/silicone rubber solid phase microextraction head was prepared by coating the polymer on the surface of Ni-Ti alloy fiber treated by potassium hydroxide hydrothermal treatment. The structure of silicone rubber was analyzed by infrared spectroscopy; The maximum using temperature of the coating was determined by thermogravimetric analysis; And the surface morphology of nickel-titanium alloy fiber wire and extraction head was observed by scanning electron microscope. The residue of acetone, tetrahydrofuran, dichloromethane and acetonitrile in western medicine was determined by headspace extraction, solid phase microextraction and gas chromatography(HS-SPME-GC). There was a good linear relationship between the peak areas and concentration of the samples, the linear correlation coefficient(R2) was 0.9916-0.9998, and the minimum detection limit was 0.058-0.235 μg/L. The standard-added recovery rate for the actual sample determination was 95.9%-99.4% and the relative standard deviation was 2.35%-3.72%.更多还原