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首页> 外文期刊>Analytical chemistry >Preparation and application of methacrylate-based cation-exchange monolithic columns for capillary ion chromatography
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Preparation and application of methacrylate-based cation-exchange monolithic columns for capillary ion chromatography

机译：基于甲基丙烯酸酯的毛细管离子色谱阳离子交换整体柱的制备及应用

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Polymer-based strong canon-exchange monolithic capillary columns with different capacities were constructed for ion chromatography by radical polymerization of glycidyl methacrylate (GMA) and ethylene dimethacrylate in a 250-mum-i.d. fused-silica capillary and its subsequent sulfonation based on ring opening of epoxides with 1 M Na2SO3. The cation-exchange capacities can easily and reproducibly be controlled in the range of up to 300 muequiv/mL by changing the immersion time of the epoxy-containing polymer in the Na2SO3 solution. The chromatographic performance of the produced monolithic capillary columns was evaluated through the separation of a model mixture of common cations such as Na+, NH4+, K+, Mg2+, and Ca2+. As an example, these cations could be well separated from one another on a 15-cm-long cation-exchange monolithic column (column volume, 7.4 muL) with a capacity of 150 muequiv/mL by elution with 10 MM CuSO4. The pressure drop of this 15-cm column was similar to1 MPa at a normal linear velocity of 1 mm/s (a flow rate of 3 muL/min), and the numbers of theoretical plates for the cations were above 3000 plates/15 cm. This GMA-based cation-exchange monolithic column could withstand high linear velocities of at least 10 mm/s. Over a period of at least two weeks of continuous use, no significant changes in the selectivity and resolution were observed. The applicability of a flow rate gradient elution and the feasibility of direct injection determination of major cations in human saliva sample were also presented.
机译：通过在250μmd.d中对甲基丙烯酸缩水甘油酯（GMA）和二甲基丙烯酸乙二酯进行自由基聚合，构建了具有不同容量的基于聚合物的强力佳能交换整体式毛细管柱，用于离子色谱法。熔融石英毛细管及其随后的磺化反应是基于环氧化物与1 M Na2SO3的开环。通过改变含环氧基的聚合物在Na2SO3溶液中的浸泡时间，可以轻松且可重复地将阳离子交换容量控制在300 muequiv / mL的范围内。通过分离常见阳离子（如Na +，NH4 +，K +，Mg2 +和Ca2 +）的模型混合物，可以评估所生产的整体式毛细管柱的色谱性能。例如，通过用10 MM CuSO4洗脱，这些阳离子可以在15 cm长的阳离子交换整体柱（柱体积，7.4μL）上以150 muequiv / mL的容量很好地相互分离。该15厘米色谱柱的压降在1毫米/秒的正常线速度（流速为3升/分钟）下类似于1兆帕，阳离子的理论塔板数超过3000板/ 15厘米。这种基于GMA的阳离子交换整体式色谱柱可承受至少10 mm / s的高线速度。在连续使用至少两周的时间内，未观察到选择性和分离度的显着变化。还介绍了流速梯度洗脱的适用性和直接进样测定人唾液样品中主要阳离子的可行性。

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