期刊
JOURNAL OF SEPARATION SCIENCE
卷 44, 期 19, 页码 3646-3653出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.202100398
关键词
3-hydroxyaspartate; capillary electrophoresis; chiral separation; microwave-assisted derivatization; online sample concentration
资金
- National Natural Science Foundation of China [21775008, 218740031, 22074003]
- Beijing Natural Science Foundation Essential Research Project [Z170002]
A chiral analytical method based on capillary electrophoresis and laser-induced fluorescence detection was developed for the simultaneous separation and detection of four stereoisomers of 3-hydroxyaspartate. By utilizing microwave-assisted derivatization and online sample concentration methods, the sensitivity was improved significantly, resulting in excellent analytical performance.
A chiral analytical method was proposed based on capillary electrophoresis with laser-induced fluorescence detection coupled with microwave-assisted derivatization for the simultaneous baseline separation and sensitive detection of four stereoisomers of 3-hydroxyaspartate. The derivatization reaction of 3-hydroxyaspartate with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole was greatly accelerated by microwave irradiation. Under the optimized conditions, the derivatization yield was increased by 20% and the derivatization time was shortened by 20 min when compared with those from conventional water bath heating. In addition, the sensitivity was improved by online sample concentration methods. The detection limit of l-threo-3-hydroxyaspartate obtained by large-volume sample stacking with polarity switching was 5.3 nmol/L, which was around 1000-fold lower than that of the capillary electrophoresis/laser-induced fluorescence without stacking. The excellent analytical performance in terms of linearity and precision was also achieved. Furthermore, the developed method was successfully applied to the determination of 3-hydroxyaspartate in the spiked urine, and satisfactory recoveries were obtained ranging from 90.5 to 107.0%.
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