How Reliable Are Enantiomeric Excess Measurements Obtained By Chiral HPLC?
How Reliable Are Enantiomeric Excess Measurements Obtained By Chiral HPLC?
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DOI：
10.1002/slct.202000166
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发表时间：
2020-02-14
期刊：
影响因子：
2.1
通讯作者：
Kass, Steven R.
中科院分区：
文献类型：
--
作者：
Payne, Curtis;Kass, Steven R.
使用 (R)- 和 (S)- 布洛芬标准品，通过不同的峰分辨率和洗脱顺序，评估通过手性柱高效液相色谱 (HPLC) 获得的对映体过量测定的不确定性和误差。每个样品进样五次，以减少数据的变异性，并且在多个波长下监测每个色谱图，以利于化学杂质的检测。使用适当的样品浓度、最有利的检测波长和默认仪器参数会导致较大的误差 (>10%)，而正确设置的积分值可提供令人印象深刻的再现性（+/- 0.5% 或更好）和准确度（
Uncertainties and errors in enantiomeric excess determinations obtained by high performance liquid chromatography (HPLC) with a chiral column are evaluated with different peak resolutions and elution orders using (R)- and (S)-ibuprofen standards. Five injections of each sample were made to reduce the variability in the data and each chromatogram was monitored at multiple wavelengths to facilitate the detection of chemical impurities. Using appropriate sample concentrations, the most favorable detection wavelengths, and default instrument parameters led to large errors (>10 %) whereas properly set integration values gave impressive reproducibilities (+/- 0.5 % or better) and accuracies (