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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Improving precision of manual hydrodynamic injection in capillary electrophoresis with contactless conductivity detection
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Improving precision of manual hydrodynamic injection in capillary electrophoresis with contactless conductivity detection

机译:通过非接触式电导检测提高毛细管电泳中手动液力注入的精度

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Reproducible injection in capillary electrophoresis has been difficult to achieve with manual injection techniques using simple injection devices, such as gravity injection (siphoning) or hydrodynamic sample splitting. We demonstrate that the injection reproducibility can be improved using very simple means. With hydrodynamic sample splitter, a passive micro-metering valve can be inserted in-line to regulate the sample flow rate through the splitter interface. A significant improvement of both reproducibility and repeatability was achieved. The reproducibility of RSD of the peak areas improved from 25.4% to 4.4%, while the repeatability was below 4.1% when micro-metering valve was used. Additional simple correction that can be used to further improve the variability of injected sample volumes in any hydrodynamic injection mode in CE with conductivity detection was proposed and verified. The measured EOF peak can serve as a simple indicator of the injected volume and can be effectively used for additional correction. By a linear function between the injection volume and the peak area of the EOF, the RSD values of peak areas for both manual gravity injection and hydrodynamic sample splitter were further improved below 2% RSD. The linearity of the calibration curve was also significantly improved. The proposed correction works even with slight differences in matrix composition, as demonstrated on the analysis aqueous soil extract of model mixture of five nerve agent degradation products.
机译:使用简单的注射装置,例如重力注射(虹吸)或流体动力学样品分裂,通过手动注射技术很难实现毛细管电泳中的可重现注射。我们证明使用非常简单的方法可以提高进样的重现性。使用流体动力学样品分配器,可将无源微量计量阀插入管线,以调节通过分离器接口的样品流速。重现性和可重复性都得到了显着改善。使用微量计量阀时,峰面积的RSD再现性从25.4%提高到4.4%,而重复性则低于4.1%。提出并验证了其他简单的校正方法,该校正方法可用于进一步改善在CE中使用电导率检测的任何流体动力学进样模式下进样量的可变性。测得的EOF峰可以用作注入量的简单指标,并且可以有效地用于其他校正。通过进样量和EOF峰面积之间的线性函数,手动重力进样和流体动力样品分流器的峰面积RSD值进一步提高到2%RSD以下。校准曲线的线性度也得到显着改善。所提出的校正方法即使在基质成分略有不同的情况下也可以正常工作,这在分析五种神经毒剂降解产物的模型混合物的土壤水提取物时得到了证明。

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