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融合核颗粒:小于2微米颗粒的实用替代物。

Fused-core particles: a practical alternative to sub-2 micron particles.

作者信息

Salisbury John J

机构信息

Analytical Research and Development, Pfizer Global Research and Development, Groton/New London Laboratories, Eastern Point Road, Groton, CT 06340, USA.

出版信息

J Chromatogr Sci. 2008 Nov-Dec;46(10):883-6. doi: 10.1093/chromsci/46.10.883.

Abstract

The benefits of sub-2 micron particle size columns have been widely researched and published. The use of these columns on ultrahigh-pressure liquid chromatography (UHPLC) instrumentation may lead to increased efficiencies and higher throughput. However, these instruments may not be readily available to the pharmaceutical chemist. Within the past year, a practical alternative has been introduced which offers increased efficiencies, but at conventional HPLC pressure limitations. These particles are called fused-core particles and are comprised of a 1.7-micron solid core encompassed by a 0.5-micron porous silica layer (dp = 2.7 micron). The goal for this research was to test these columns for efficiency and robustness utilizing a mixture of Torcetrapib and its relative impurities. Our results indicate that excellent theoretical plates (approximately 14000) were achievable for run times less than 5 min. Compared to the Waters Acquity particles, the fused-core particles achieved approximately 80% of the efficiency but with half the observed backpressure. Our robustness results concluded that these separations were reproducible for at least 500 injections while the % RSD for retention time, theoretical plates, peak asymmetry, and resolution was found to be less than 1%.

摘要

亚2微米粒径色谱柱的优势已得到广泛研究并发表。在超高压液相色谱(UHPLC)仪器上使用这些色谱柱可能会提高效率并实现更高的通量。然而,药物化学家可能无法轻易获得这些仪器。在过去的一年里,一种实用的替代方法被引入,它能提高效率,但压力限制在传统HPLC范围内。这些颗粒被称为融合核颗粒,由一个1.7微米的实心核和一个0.5微米的多孔二氧化硅层(dp = 2.7微米)组成。本研究的目的是利用托彻普(Torcetrapib)及其相关杂质的混合物来测试这些色谱柱的效率和耐用性。我们的结果表明,对于运行时间少于5分钟的情况,可以实现优异的理论塔板数(约14000)。与沃特世(Waters)Acquity颗粒相比,融合核颗粒的效率约为其80%,但观察到的背压仅为其一半。我们的耐用性结果表明,这些分离至少在500次进样时具有可重复性,同时保留时间、理论塔板数、峰不对称性和分离度的相对标准偏差(%RSD)小于1%。

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