Photopolymerized sol-gel frits for packed columns in capillary electrochromatography.
Photopolymerized sol-gel frits for packed columns in capillary electrochromatography.
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DOI：
10.1016/s0021-9673(01)00772-5
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发表时间：
2001-07
期刊：
影响因子：
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通讯作者：
M. Kato;M. Dulay;Bryson D. Bennett;J. Quirino;Richard N. Zare
中科院分区：
文献类型：
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作者：
M. Kato;M. Dulay;Bryson D. Bennett;J. Quirino;Richard N. Zare
在毛细管柱中通过填充甲基丙烯酸3-（三甲氧基甲硅烷基）丙酯、盐酸、水、甲苯（致孔剂）和光引发剂（Irgacure 1800）的溶液并将其暴露于365 nm的紫外光下5 min来制备多孔溶胶-凝胶熔块。在入口和出口玻璃料之间包含一个15 cm填充段，填充有用手性化合物（S）-N-3，5-二硝基苯甲酰基-1-萘基甘氨酸改性的5 μm二氧化硅颗粒。在出口玻璃料之后立即放置检测窗（1 mm长）。为了证明该手性分离柱的性能，用荧光试剂4-氟-7-硝基-2，1，3-苯并恶二唑衍生的16种不同氨基酸（其中三种不是天然存在的）的混合物通过毛细管色谱法分离。对映体的分离度为1.21 ~ 8.29，塔板高度为8.7 ~ 39 μm。
Porous sol–gel frits are fabricated in a capillary column by filling it with a solution of 3-(trimethoxysilyl)propyl methacrylate, hydrochloric acid, water, toluene (porogen), and a photoinitiator (Irgacure 1800) and exposing it to UV light at 365 nm for 5 min. The separation column (30 cm×75 μm I.D.) contains between the inlet and outlet frits a 15-cm packed segment filled with 5-μm silica particles modified with the chiral compound (S)-N-3,5-dinitrobenzoyl-1-naphthylglycine. A detection window (1 mm long) is placed immediately after the outlet frit. To demonstrate the performance of this chiral separation column, mixtures of 16 different amino acids (three of which are not naturally occurring) derivatized with the fluorogenic reagent 4-fluoro-7-nitro-2,1,3-benzoxadiazole were separated by capillary chromatography. The enantiomeric separation of the column results in a resolution ranging from 1.21 to 8.29, and a plate height ranging from 8.7 to 39 μm.