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- W2894870609 abstract "A new analytical method based on capillary zone electrophoresis-mass spectrometry (CZE-MS) was proposed and validated for the simultaneous determination of four stereoisomers of 3-hydroxyaspartate with two chiral centers in rat cerebrospinal fluid (CSF) in absence of optically pure single enantiomer standards. The derivatization reagent 9-fluorenylmethyl chloroformate (FMOC-Cl) was found to assist chiral separation and the derivatized enantiomers of 3-hydroxyaspartate can achieve enantioseparation with a lower concentration (6 mM) of β-cyclodextrin (β-CD), while underivatized 3-hydroxyaspartate cannot be separated. The enhanced interactions between derivatized analytes and β-CD were demonstrated by proton nuclear magnetic resonance (1H NMR). The four stereoisomers of FMOC-3-hydroxyaspartate were identified successfully using a new method based on experimental and calculated electronic circular dichroism (ECD) spectra combined with the comparison of CE peak areas. Large volume sample stacking with polarity switching (LVSS-PS) was used to increase sensitivity and the detection limit of 356 nM was achieved for L-THA, which was around 10-fold improvement compared to the normal CE-MS analysis. The composition of the background electrolyte (BGE) was optimized by response surface methodology (RSM). Under the optimal conditions, satisfactory results of L-THA were obtained in terms of linearity over the range of 2–80 μM (R2 > 0.99) and precision (RSD below 1.43% and 2.56% for migration time and peak area, respectively). The recoveries for all four stereoisomers in spiked rat CSF ranged from 91.2% to 99.5%. The method has been successfully applied to rat CSF analysis and D-erythro-3-hydroxyaspartate (D-EHA) was detected." @default.
- W2894870609 created "2018-10-12" @default.
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- W2894870609 date "2019-01-01" @default.
- W2894870609 modified "2023-09-26" @default.
- W2894870609 title "Derivatization reagent-assisted enantioseparation of 3-hydroxyaspartate with two chiral centers in rat cerebrospinal fluid by capillary electrophoresis-mass spectrometry" @default.
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- W2894870609 doi "https://doi.org/10.1016/j.aca.2018.09.070" @default.
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