Ni-Ti丝基体固相微萃取头的制作及其在样品分析中的应用

Preparation of Ni-Ti wire matrix solid phase microextraction head and its application in sample analysis

以四氢呋喃-N,N-二甲基甲酰胺为混合溶剂,均苯四甲酸二酐、二苯甲酮四羧酸二酐、二氨基二苯基醚(ODA)、氨丙基封端聚二甲基硅氧烷为原料,制备聚酰胺酸,涂渍到经碱水热处理的镍钛合金纤维丝表面,经高温脱水环化生成聚酰亚胺聚硅氧烷,从而得到金属丝基体涂渍聚合物固相微萃取头.采用红外光谱法分析涂层结构,热重分析法测定聚酰亚胺聚硅氧烷的分解温度,通过扫描电子显微镜观察制备的萃取头的表面形貌.通过顶空萃取-固相微萃取-气相色谱质谱联用(HS-SPME-GC/MS)法对白酒中挥发性物质的分析,考察了涂层的吸附选择性,透过重复性实验考察了萃取头的耐用性.

Take tetrahydrofuran-N,N-dimethylformamide as the mixed solvent,pyromelliticdianhydride,benzophenone tetracarboxylicdianhydride,diaminodiphenyl ether(ODA)and aminopropyl terminated polydimethylsiloxane as raw materials,prepared polyamic acid and coated on the surface of NiTi alloy fiber after alkali hydrothermal treatment.Polyimide polysiloxane was synthesized by dehydration and cyclization at high temperature,and the polymer solid phase microextraction head coated on metal wire was obtained.The structure of the coating was analyzed by infrared spectroscopy,the decomposition temperature of polyimide polysiloxane was determined by thermogravimetric analysis,and the surface morphology of the extraction head was observed by scanning electron microscope.Headspace extraction solid phase microextractioncoupled with gas chromatography mass spectrometry(HS-SPME-GC/MS)was used to analyze the volatile compounds in Baijiu,and the adsorption selectivity of the coating was investigated.The durability of the extraction head was investigated through repeated experiments.