Chen Tao, Fan Jun, Gao Ruiqi, Wang Tai, Yu Ying, Zhang Weiguang
School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
J Chromatogr A. 2016 Oct 7;1467:246-254. doi: 10.1016/j.chroma.2016.07.007. Epub 2016 Jul 5.
Chiral stationary phase-high performance liquid chromatography coupled with various detectors has been one of most commonly used methods for analysis and separation of chiral compounds over the past decades. Various detectors exhibit different characteristics in qualitative and quantitative studies under different chromatographic conditions. Herein, a comparative evaluation of HPLC coupled with ultraviolet, optical rotation, refractive index, and evaporative light scattering detectors has been conducted for qualitative and quantitative analyses of metalaxyl racemate. Effects of separation conditions on the peak area ratio between two enantiomers, including sample concentration, column temperature, mobile phase composition, as well as flow rate, have been investigated in detail. In addition, the limits of detection, the limits of quantitation, quantitative range and precision for these two enantiomers by using four detectors have been also studied. As indicated, the chromatographic separation conditions have been slight effects on ultraviolet and refractive index detections and the peak area ratio between two enantiomers remains almost unchanged, but the evaporative light scattering detection has been significantly affected by the above-mentioned chromatographic conditions and the corresponding peak area ratios varied greatly. Moreover, the limits of detection, the limits of quantitation, and the quantitative ranges of two enantiomers with UV detection were remarkably lower by 1-2 magnitudes than the others.
在过去几十年中,手性固定相高效液相色谱结合各种检测器一直是分析和分离手性化合物最常用的方法之一。在不同的色谱条件下,各种检测器在定性和定量研究中表现出不同的特性。在此,对手性甲霜灵外消旋体进行了高效液相色谱结合紫外、旋光、折光率和蒸发光散射检测器的定性和定量分析的比较评估。详细研究了分离条件对两种对映体峰面积比的影响,包括样品浓度、柱温、流动相组成以及流速。此外,还研究了使用四种检测器对这两种对映体的检测限、定量限、定量范围和精密度。结果表明,色谱分离条件对紫外和折光率检测影响较小,两种对映体的峰面积比几乎保持不变,但蒸发光散射检测受到上述色谱条件的显著影响,相应的峰面积比变化很大。此外,紫外检测的两种对映体的检测限、定量限和定量范围比其他检测方法低1-2个数量级。