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High sensitivity deep-UV LED-based z-cell photometric detector for capillary liquid chromatography

机译:基于高灵敏度的深紫外LED基Z细胞光度检测器,用于毛细管液相色谱法

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A new high sensitivity deep-UV LED photometric detector with a z-type flow cell (45?nL or 180?nL) for miniaturised and portable capillary liquid chromatography (LC) was designed and fabricated to overcome sensitivity limitations due to short pathlength in on-capillary detectors. The new detector has a 10?mm geometric pathlength and uses high intensity light-emitting diodes (LED) as light sources in the deep-UV range (254?nm and 280?nm). No optical reference was necessary due to the low drift in the signal. Stray light was minimized by the use of an adjustable slit with a 0.5?mm pinhole. The direct relationship between absorbance and concentration was obtained using dichromate to evaluate the sensitivity and the linearity range of the detector. Performance of the miniaturised version was compared with that obtained from a commercial benchtop detector for capillary LC under the same conditions using the same optical z-cell. The miniaturised version exhibited a superior performance across all parameters, including 3 times higher effective pathlength, 4 times higher upper limit of detector linearity, and 2–5 times lower stray light levels. An application of the new detector was shown with the detection ofl-dopa,l-tyrosine, norfenefrine, phenylephrine and tyramine, separated using capillary LC. The baseline noise level recorded was as low as 3.9 μAU. Further, the detector was applied in a miniaturised capillary LC for the indirect detection of common inorganic anions. In comparison to an on-capillary LED detector applied under similar chromatographic conditions, there was a 50 times higher signal to noise (S/N) ratio.
机译:设计并制造具有用于小型化和便携式毛细管液相色谱(LC)的Z型流通池(45〜N1或180〜N1)的新型高灵敏度深紫外线LED光度检测器,以克服由于较短的路径通道而克服灵敏度限制-capillary探测器。新探测器具有10?MM几何路径长度,并使用高强度发光二极管(LED)作为深紫色范围(254Ω·NM和280Ω)的光源。由于信号中的低漂移,不需要光学参考。通过使用具有0.5Ω大针孔的可调节狭缝,最小化杂散光。使用二分甲酸酯获得吸光度和浓度之间的直接关系,以评估检测器的灵敏度和线性范围。将小型化版本的性能与使用相同光学Z细胞的相同条件下的毛细管LC的商业台式探测器获得的性能。小型化版本在所有参数中表现出卓越的性能,包括3倍的有效程度,检测器线性上限的4倍,杂散光线下降2-5倍。显示了新探测器的应用,检测到DOPA,L-酪氨酸,NORFENEFRINE,NORFENEFRINE,苯妥和酪胺,使用毛细管LC分离。记录的基线噪声水平低至3.9μAU。此外,检测器应用于小型化毛细管LC,用于间接检测常见的无机阴离子。与在相似的色谱条件下施加的上毛细管LED检测器相比,信号噪声(S / N)比率越高的50倍。

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