改質不銹鋼絲表面鍵結聚離子液體作為固相微萃取測定環境水樣品中的防腐劑含量

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標題:	改質不銹鋼絲表面鍵結聚離子液體作為固相微萃取測定環境水樣品中的防腐劑含量 Grafting of Polyionic Liquid on Modification Stainless Steel Wire Surface as Solid Phase Microextraction for Preservatives in Environment Water Sample
作者:	呂宛諭
貢獻者:	化粧品應用與管理系林維炤
關鍵字:	不銹鋼聚離子液體固相微萃取氣相層析質譜儀防腐劑 stainless steel poly ionic liquid solid phase microextraction gas chromatography mass spectrometer preservative
日期:	2018
上傳時間:	2019-02-27 16:51:39 (UTC+8)
摘要:	本研究以覆載於不銹鋼絲上的聚離子液體作為吸附靜相，以固相微萃取方式測定水中防腐劑。首先利用1-乙烯基咪唑與1-溴辛烷進行烷基化反應，合成溴化咪唑鹽(支鏈型離子液體)；利用咪唑與1-溴-6-氯己烷進行烷基化反應，其次在乙二醇中進行自聚合反應後加入1-乙烯基咪唑進行高分子末端基修飾(支鏈-主鏈型離子液體)。接著與雙三氟甲烷硫磺醯亞胺化鋰進行離子交換，即可製備出陰離子NTf2- 的聚離子液體。離子液體借著改質不銹鋼表面上的矽烷類化合物與進行接合，偶氮二異丁?為起始劑進行自由基鍵結反應，為自製的固相微萃取(SPME)靜相纖維。結合氣相層析質譜儀(GC-MS)測定在環境水中八種防腐劑成分。水樣中添加乙酸酐進行醯化衍生，使反應是將結構上的羥基衍生成酯類，以提升分析物之揮發性，再利用自製之SPME以頂空方式進行水中防腐劑測定。實驗結果顯示，沾取10~15次膜厚約11.7~16.2?m；防腐劑衍生化水樣調整pH值為9.0、添加35% 的NaCl、溫度以80℃下反應30分鐘、吸附50分鐘，有較佳的萃取效果。同日異日分析回收率範圍介於89.7±29.0% ~139.7±38.8%；方法偵測極限介於2.13~12.12ng/mL。 This study is to investigate the preservative in water by solid phase microextraction using poly ionic liquid coated on stainless steel.The polymeric ionic liquids(PILs) systhesis steps was following, the alkylation of 1-vinyl imidazole with 1-bromooctane (Side chain ILs) / the imidazole reacted with 1-bromo-6-chlorohexane to form the monomer first. The monomers were placed in ethylene glycol for self-polymerization, then 1-vinylimidazole was added for terminal group modification. Lithium bis (trifluoromethanesulfon) imide was added for anion exchange. The ionic liquid (ILs) were grafted by a decane compound on the surface of the modified stainless steel. Azobisisobutyronitrile as a starting agent for free radical bonding reaction, for self-made solid phase microextraction (SPME) stationary phase fibers.Eight preservatives in water by solid phase microextraction and determination by gas chromatography mass spectrometry. The self-made SPME was used to determine the preservative in water in the headspace, and the water sample was added with acetic anhydride. The reaction is to derivatize the structural hydroxyl groups to esters to increase the volatility of the analyte for deuteration to increase the volatility of the analyte.The ionic liquid film is conducted by dipping stainless fiber in acetone containing ionic liquid. The film thickness is around 11.7-16.2?m after 5-20 times dip. For the derivative steps, the optimum condition is reached at 80 ? C for 30 minutes. The headspace solid phase microextraction is performed by 35% NaCl is added, water is adjusted to pH 9.0, and adsorption is carried out for 50 minutes.The stainless fiber coated ionic liquid is put on the headspace of water in a 20 mL vials, the optimum extraction is found at 80? C for fifty minutes. Same day analysis and recovery rate range 89.7 ? 29.0% ~139.7 ? 38.8%. Detection limit is between 2.13~12.12ng/mL.
關聯:	電子全文公開日期：2023-07-31，學年度：106， 91頁
顯示於類別:	[化妝品應用與管理系(所)] 博碩士論文

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