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Cavity ring-down spectroscopy as a detector for liquid chromatography

机译:腔衰荡光谱作为液相色谱检测器

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We have demonstrated the use of cavity ring-down spectroscopy (CRDS) as a detector for high performance liquid chromatography (HPLC). For this use, we have designed and implemented a Brewster's angle flow cell such that cavity ring-down spectroscopy can be performed on microliter volumes of liquids. The system exhibits a linear dynamic range of 3 orders of magnitude (30 nM to 30,muM quinalizarin at 470 nm) for static measurements and 2 orders of magnitude (0.5 muM to 50 muM) for HPLC measurements. For the static measurements, the baseline noise is 2.8 x 10(-6) AU rms and 1.0 x 10(-5) AU peak-to-peak, and for the HPLC separations, it is 3.2 x 10(-6) AU rms and 1.3 x 10(-5) AU peak-to-peak. The baseline noise is determined after the data are smoothed by an 11-point boxcar average. The peak areas detected from HPLC separations are reproducible to within 2-3%. The HPLC mass detection limit for a molecule with epsilon = 9 x 10(3) M-1 cm(-1) in a 300-mum path length cell (illuminated volume, 0.5 muL) is reported as 2.5 x 10(-8) g/mL. These results were obtained using a simple pulsed CRDS system and are comparable to, if not better than, a high-quality commercial UV-vis absorption detector for the same path length. [References: 30]
机译:我们已经证明了使用腔衰荡光谱(CRDS)作为高效液相色谱(HPLC)的检测器。为此,我们设计并实现了布鲁斯特角流通池,以便可以对微升体积的液体进行腔衰荡光谱分析。对于静态测量,该系统的线性动态范围为3个数量级(在470 nm处为30 nM至30,μM喹那扎林),对于HPLC测量,该系统具有2个数量级(0.5μM至50μM)。对于静态测量,基线噪声为2.8 x 10(-6)AU rms和1.0 x 10(-5)AU峰-峰,而对于HPLC分离,则为3.2 x 10(-6)AU rms和1.3 x 10(-5)AU峰峰值。在通过11点棚车平均值对数据进行平滑处理后,确定基线噪声。从HPLC分离中检测到的峰面积可重现2-3%。在300微米路径长度的小室中,epsilon = 9 x 10(3)M-1 cm(-1)的分子的HPLC质量检测限据报道为2.5 x 10(-8)(照明体积为0.5μL)克/毫升。这些结果是使用简单的脉冲CRDS系统获得的,即使在相同的路径长度下也可以与高质量的商用UV-vis吸收检测器相媲美,甚至更好。 [参考:30]

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