本文選題：親水作用色譜 + 磺酸甜菜堿�。� 參考：《寧夏大學(xué)》2017年碩士論文

【摘要】：本文以色譜硅膠為基質(zhì),采用原子轉(zhuǎn)移自由基聚合(ATRP)技術(shù)將合成的N,N-二甲基-N-丙烯酰氧乙基-N-丙基磺酸銨(DMAEAPS)和N-乙烯基咪唑-N-丙磺酸鹽(VIMPS)兩種兩性離子功能單體分別鍵合到Sil-Br基質(zhì)材料表面,制備出含DMAEAPS和VIMPS的兩種不同的磺酸甜菜堿型兩性離子Sil-DMAEAPS和Sil-VIMPS色譜填料,通過考察極性溶質(zhì)在自制色譜固定相上的保留行為,研究其色譜性能。同時考察了鹽效應(yīng)對不同極性溶質(zhì)在硅膠柱(Kinetex silica)、氨基柱(Luna NH2)、烷基甜菜堿型兩性離子柱(ZIC(?)-HILIC)、磷酰膽堿改性硅膠柱(ZIC(?)-cHILIC)四種商品柱上保留行為的影響,得到了一些有價值的結(jié)論。如以下幾個部分:1.以丙烯酸二甲氨基乙酯(DMAEA)和1,3-丙磺酸內(nèi)酯為原料,合成了含磺酸甜菜堿型兩性離子的功能單體NN-二甲基-N-丙烯酰氧乙基-N-丙基磺酸銨(DMAEAPS),通過ATRP技術(shù)將其接枝到Sil-Br表面,制備出含DMAEAPS功能單體的Sil-DMAEAPS磺酸甜菜堿型兩性離色譜固定相。研究了該固定相對安息香、維生素B6、蕓香葉苷、對香豆酸和咖啡酸5種極性溶質(zhì)的親水作用色譜分離性能,發(fā)現(xiàn)極性溶質(zhì)在典型的親水作用色譜條件下(乙腈:水0.7,v/v),其保留主要由靜電作用和親水作用控制,而在典型的反相色譜條件下(乙腈:水0.2,v/v),則表現(xiàn)出反相柱的分離特征,極性溶質(zhì)在該固定相上的保留是親水色譜與反相色譜相結(jié)合的混合機理。與ZIC(?)-HILIC商品柱進行對比,發(fā)現(xiàn)自制色譜柱對溶質(zhì)表現(xiàn)出不同的分離選擇性。將自制色譜柱用于蘆丁片中蕓香葉苷以及當歸、升麻中阿魏酸含量的測定,操作方法簡單,為極性樣品的分離提供了新方法。2.在冰浴磁力攪拌條件下以N-乙烯基咪唑和1,3-丙磺酸內(nèi)酯為原料反應(yīng)8 h,合成了N-乙烯基咪唑-N-丙磺酸鹽兩性離子(VIMPS)功能單體,采用1H-NMR及FT-IR對功能單體進行了表征。通過ATRP技術(shù)將VIMPS功能單體接枝到Sil-Br引發(fā)劑上,制備出含VIMPS功能單體的磺酸甜菜堿型兩性離子(Sil-VIMPS)色譜固定相,通過元素分析,得知成功制備出Sil-VIMPS色譜填料。選取維生素B1、安息香、維生素B6、葛根素、阿魏酸、對香豆酸、咖啡酸、綠原酸8種酸堿性不同的極性溶質(zhì),以乙腈/甲酸銨緩沖鹽為流動相,通過調(diào)節(jié)流動相甲酸銨緩沖鹽濃度、乙腈含量、pH值,考察了極性溶質(zhì)在該色譜固定相上的保留情況,實驗結(jié)果表明所合成的Sil-VIMPS色譜固定相呈現(xiàn)出較優(yōu)的親水性及靜電作用,對強堿性及酸性溶質(zhì)均有良好的分離選擇性。3.鹽效應(yīng)對改變HILIC的選擇性有重要作用,通過改變緩沖鹽種類、鹽濃度等條件,系統(tǒng)地研究了尿嘧啶、尿嘧啶核苷、腺嘌呤、腺嘌呤核苷、胞嘧啶、胞嘧啶核苷、安息香、青霉素、維生素B6、阿魏酸、煙酸、咖啡酸和綠原酸等極性溶質(zhì)組分在Kinetex silica、Luna NH2、ZIC(?)-HILIC、ZIC(?)-cHILIC上的保留行為。結(jié)果發(fā)現(xiàn),甲酸銨緩沖鹽濃度對極性溶質(zhì)保留的影響較大,而硫酸銨緩沖鹽的濃度對極性溶質(zhì)的保留影響較小。
[Abstract]:In this paper, N, N- two methyl -N- acryl -N- propyl -N- propyl sulfonate (DMAEAPS) and N- vinyl imidazole -N- propane sulfonate (VIMPS) two kinds of amphoteric ionic functional monomers were bonded to the surface of Sil-Br matrix material by atomic transfer radical polymerization (ATRP), and two species containing DMAEAPS and VIMPS were prepared. The chromatographic performance of different sulfonated betaine type amphoteric ions Sil-DMAEAPS and Sil-VIMPS chromatography was investigated by investigating the retention behavior of polar solute on the homemade chromatographic stationary phase. At the same time, the effect of salt effect on different polar solutes in silica gel column (Kinetex silica), amino column (Luna NH2), alkyl betaine type amphoteric ion column (ZIC (?)) was investigated. HILIC), some valuable conclusions were obtained from the influence of the retention behavior of four kinds of silica gel column (ZIC (?) -cHILIC) on the silica gel column (ZIC (?) -cHILIC). For example, the functional monomer NN- two methyl -N- acryl containing sulfonate betaine type amphoteric ions was synthesized by using two methylamino ethyl acrylate (DMAEA) and 1,3- propionate lactate as raw materials. Oxygen ethyl -N- propyl sulfonic acid (DMAEAPS) was grafted onto the surface of Sil-Br by ATRP technology to prepare a Sil-DMAEAPS sulfonic acid betaine type separation chromatographic stationary phase containing DMAEAPS functional monomers. The hydrophilic chromatographic separability of the fixed relative benzoin, vitamin B6, rutin, and 5 polar solutes of coumaric acid and caffeic acid were studied. It is found that the polar solute is under the typical hydrophilic interaction chromatography (acetonitrile: water 0.7, v/v), and its retention is controlled mainly by electrostatic action and hydrophilic action, while the typical reverse phase chromatography (acetonitrile: water 0.2, v/v) shows the separation characteristics of the reverse phase column, and the retention of polar solute on the stationary phase is the hydrophilic and reverse phase chromatography Compared with the ZIC (?) -HILIC column, it was found that the homemade chromatographic column showed different separation selectivity for the solute. The homemade chromatographic column was used for the determination of the rutoside and Angelica in Rutinum Tablets, the determination of ferulic acid content in the cohosh, simple operation method, and a new method,.2. in the ice bath magnetic force for the separation of polar samples. The N- vinyl imidazole -N- propanosulfonate amphoteric ion (VIMPS) functional monomer was synthesized with N- vinyl imidazole and 1,3- propionate as raw material under stirring conditions, and the functional monomers were characterized by 1H-NMR and FT-IR. The sulfonium containing VIMPS functional monomers was grafted onto Sil-Br initiator by ATRP technology, and the sulfonated monomers containing the VIMPS functional monomer were prepared. Acid betaine type amphoteric ion (Sil-VIMPS) chromatography fixed phase, through the element analysis, the Sil-VIMPS chromatographic packing was successfully prepared. Vitamin B1, benzoin, vitamin B6, puerarin, ferulic acid, and 8 kinds of acid and alkali solute with different acids and alkalinity of coumaric acid, caffeic acid and chlorogenic acid, acetonitrile / ammonium formate buffer salt was used as the mobile phase, through regulating flow. The concentration of ammonium formate buffer salt, the content of acetonitrile, pH value, and the retention of polar solute on this chromatographic stationary phase were investigated. The experimental results showed that the synthesized Sil-VIMPS chromatographic stationary phase showed better hydrophilic and electrostatic effect, and good separation and selective.3. salt efficiency for strong alkaline and acidic solutes should be selected to deal with the selection of HILIC. Selectivity has an important role in the systematic study of uracil, uracil, adenine, adenine, adenine, cytosine, cytosine, cytosine, cytosine, cytosine, cytosine, vitamin B6, ferulic acid, nicotinic acid, chlorogenic acid and chlorogenic acid in Kinetex silica, Luna NH2, ZIC (?) -HILIC, ZIC. (?) retention behavior on -cHILIC. It is found that the concentration of ammonium formate buffer salt has great influence on the retention of polar solute, while the concentration of ammonium sulfate buffer salt has little effect on the retention of polar solute.
【學(xué)位授予單位】：寧夏大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O652.6

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