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基于聚甲基辛基硅氧烷固定在硅胶上的固定相的硅醇活性的碱性溶质的色谱评估。

Chromatographic evaluation using basic solutes of the silanol activity of stationary phases based on poly(methyloctylsiloxane) immobilized onto silica.

机构信息

Institute of Chemistry, University of Campinas, Campinas, SP, Brazil.

出版信息

J Sep Sci. 2011 May;34(10):1141-8. doi: 10.1002/jssc.201000700. Epub 2011 Apr 13.

Abstract

The chromatographic behaviors of some basic solutes were evaluated on stationary phases based on poly(methyloctylsiloxane) immobilized onto silica (PMOS-SiO(2)). The test solutes present both hydrophobic and hydrophilic properties. Evaluations of the pH effect used 80:20 v/v methanol/buffered mobile phase over the pH range of 5-11.5 with inorganic buffers such as borate, carbonate and phosphate and with organic buffers such as citrate, tricine and triethylamine. Evaluations in acidic mobile phases used 50:50 v/v and 30:70 v/v methanol/buffer (pH 2.5; 20 mmol/L) mobile phases. The buffer concentration effect used 65:35 v/v methanol/phosphate (pH 7; 20 and 100 mmol/L) mobile phases. The results are compared with those obtained with two chemically bonded stationary phases. The immobilized phases show greater contributions from an ion-exchange mechanism than do the commercial phases. The results indicate that the silanol activity of PMOS-SiO(2) stationary phases can be adequately evaluated by using appropriate basic probes and mobile phases having different pH, using different buffers.

摘要

采用固定在硅胶上的聚甲基辛基硅氧烷(PMOS-SiO2)为固定相,评价了一些碱性溶质的色谱行为。这些测试溶质具有疏水性和亲水性。考察 pH 值的影响时,使用 80:20v/v 甲醇/缓冲流动相,pH 值范围为 5-11.5,缓冲液为硼酸盐、碳酸盐和磷酸盐等无机缓冲液,以及柠檬酸盐、三羟甲基氨基甲烷和三乙胺等有机缓冲液。在酸性流动相中,使用 50:50v/v 和 30:70v/v 甲醇/缓冲液(pH 2.5;20mmol/L)作为流动相。考察缓冲液浓度的影响时,使用 65:35v/v 甲醇/磷酸盐(pH 7;20 和 100mmol/L)作为流动相。将结果与两种化学键合固定相的结果进行了比较。固定相表现出比商业固定相更大的离子交换机制贡献。结果表明,采用适当的碱性探针和具有不同 pH 值的不同缓冲液,可以用合适的碱性探针和不同 pH 值的不同缓冲液来充分评价 PMOS-SiO2 固定相的硅醇活性。

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