Derivatization reagent-assisted enantioseparation of 3-hydroxyaspartate with two chiral centers in rat cerebrospinal fluid by capillary electrophoresis-mass spectrometry

Liu, Mingxia; Zhao, Hong; Zhang, Zhiguo; Li, Xiangjun; Mao, Lanqun; Zhang, Ruiping; Wang, Yuekui

doi:10.1016/j.aca.2018.09.070

Cited by 20 publications

(26 citation statements)

References 57 publications

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“…However, CE with absorbance detection showed relatively poor sensitivity, because of the limited optical pathway of on‐capillary photometry and the small sample injection volume. In order to enhance detection sensitivity of CE‐UV, several online enrichment technologies have been established, such as stacking , sweeping , solid‐phase packing , and transient trapping technique . Pressure‐assisted electrokinetic injection (PAEKI) as an online enhancement technique has been proposed to provide a powerful enhancement capability without compromising the separation efficiency .…”

Section: Introductionmentioning

confidence: 99%

Dispersive liquid‐liquid microextraction coupled with pressure‐assisted electrokinetic injection for simultaneous enrichment of seven phenolic compounds in water samples followed by determination using capillary electrophoresis

Gao

Lü

et al. 2019

J of Separation Science

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Offline dispersive liquid-liquid microextraction combined with online pressureassisted electrokinetic injection was developed to simultaneously enrich seven phenolic compounds in water samples, followed by determination using capillary electrophoresis, namely phenol, 4-chlorophenol, pentachlorophenol, 2,4,6trichlorophenol, 2,4-dichlorophenol, 2-chlorophenol, and 2,6-dichlorophenol. Several parameters affecting separation performance of capillary electrophoresis and the enrichment efficiency of pressure-assisted electrokinetic injection and dispersive liquid-liquid microextraction were systematically investigated. Under the optimal conditions, seven phenolic compounds were completely separated within 14 min and good enrichment factors were obtained of 61, 236, 3705, 3288, 920, 86, and 1807 for phenol, 4-chlorophenol, pentachlorophenol, 2,4,6-trichlorophenol, 2,4-dichlorophenol, 2-chlorophenol, and 2,6-dichlorophenol, respectively. Good linearity was attained in the range of 0.1-200 μg/L for 2,4-dichlorophenol, 0.5-200 μg/L for 4-chlorophenol, pentachlorophenol, 2,4,6-trichlorophenol, 2-chlorophenol, and 2,6-dichlorophenol, as well as 1-200 μg/L for phenol, with correlation coefficients (r) over 0.9905. The limits of detection and quantification ranging from 0.03-0.28 and 0.07-0.94 μg/L were attained. This two step enrichment method was potentially applicable for the rapid and simultaneous determination of phenolic compounds in water samples. K E Y W O R D Scapillary electrophoresis, dispersive liquid-liquid microextraction, phenolic compounds, pressure-assisted electrokinetic injection, water samples

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Section: Introductionmentioning

confidence: 99%

Dispersive liquid‐liquid microextraction coupled with pressure‐assisted electrokinetic injection for simultaneous enrichment of seven phenolic compounds in water samples followed by determination using capillary electrophoresis

Gao

Lü

et al. 2019

J of Separation Science

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“…Liu et al. [51] employed BBD for the separation of 3‐hydroxyaspartate enantiomers; the evaluated responses were the peak resolution and area, and the studied factors were the concentrations of the chiral selector and BGE and the organic modifier content. The assessment of the peak area was significant because the authors employed CE coupled with mass spectrometry (CE–MS).…”

Section: Optimization Designsmentioning

confidence: 99%

“…BBD was successfully employed to optimize the enantioselective methods for the analysis of the enantiomeric purities of the chiral drug, cinacalcet (CIN) [50], and the nonproteogenic amino acid, 3-hydroxyaspartate, in rat cerebrospinal fluid [51]. For the optimization step, the authors of the previously cited work [50] studied the following factors: pH of BGE, the concentration of cyclodextrin, the methanol content of BGE, and voltage.…”

Section: Bbdmentioning

confidence: 99%

An appraisal of experimental designs: Application to enantioselective capillary electromigration techniques

2021

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Enantioresolution processes are vital tools for investigating the enantioselectivities of chiral compounds. An analyst resolves to optimize enantioresolution conditions once they are determined. Generally, optimization is conducted by a one-factor-at-a-time (OFAT) approach. Although this approach may determine an adequate condition for the method, it does not often allow the estimation of the real optimum condition. Experimental designs are conducive for the optimization of enantioresolution methods via capillary electromigration techniques (CETs). They can efficiently extract information from the behavior of a method and enable the estimation of the real optimum condition. Furthermore, the application of the analytical quality by design (AQbD) approach to the development of CETbased enantioselective methods is a trend. This article (i) offers an overview of the application of experimental designs to the development of enantioselective methods from 2015 to mid-2020, (ii) reveals the experimental designs that are presently employed in CET-based enantioresolutions, and (iii) offers a critical point of view on how the different experimental designs can aid the optimization of enantioresolution processes by considering the method parameters.

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“…Depending on their nature and concentration (stable crown-ether complexes being one exception [270]), PSPs can significantly suppress the ionization of the analytes of interest, leading to severe loss of sensitivity and inaccurate (semi-)quantitative results. Suppression of the EOF or lowering the concentration of the chiral selector can minimize these issues [271,272], although without completely eliminating them. The partialfilling technique (PFT) and the counter-migration technique (CMT) are possible approaches to overcome these issues.…”

Section: Chiral Ekc-msmentioning

confidence: 99%

Past, present, and future developments in enantioselective analysis using capillary electromigration techniques

2020

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Past, present, and future developments in enantioselective analysis using capillary electromigration techniques Enantioseparation of chiral products has become increasingly important in a large diversity of academic and industrial applications. The separation of chiral compounds is inherently challenging and thus requires a suitable analytical technique that can achieve high resolution and sensitivity. In this context, CE has shown remarkable results so far. Chiral CE offers an orthogonal enantioselectivity and is typically considered less costly than chromatographic techniques, since only minute amounts of chiral selectors are needed. Several CE approaches have been developed for chiral analysis, including chiral EKC and chiral CEC. Enantioseparations by EKC benefit from the wide variety of possible pseudostationary phases that can be employed. Chiral CEC, on the other hand, combines chromatographic separation principles with the bulk fluid movement of CE, benefitting from reduced band broadening as compared to pressure-driven systems. Although UV detection is conventionally used for these approaches, MS can also be considered. CE-MS represents a promising alternative due to the increased sensitivity and selectivity, enabling the chiral analysis of complex samples. The potential contamination of the MS ion source in EKC-MS can be overcome using partial-filling and counter-migration techniques. However, chiral analysis using monolithic and open-tubular CEC-MS awaits additional method validation and a dedicated commercial interface. Further efforts in chiral CE are expected toward the improvement of existing techniques, the development of novel pseudostationary phases, and establishing the use of chiral ionic liquids, molecular imprinted polymers, and metalorganic frameworks. These developments will certainly foster the adoption of CE(-MS) as a well-established technique in routine chiral analysis.

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Derivatization reagent-assisted enantioseparation of 3-hydroxyaspartate with two chiral centers in rat cerebrospinal fluid by capillary electrophoresis-mass spectrometry

Cited by 20 publications

References 57 publications

Dispersive liquid‐liquid microextraction coupled with pressure‐assisted electrokinetic injection for simultaneous enrichment of seven phenolic compounds in water samples followed by determination using capillary electrophoresis

Dispersive liquid‐liquid microextraction coupled with pressure‐assisted electrokinetic injection for simultaneous enrichment of seven phenolic compounds in water samples followed by determination using capillary electrophoresis

An appraisal of experimental designs: Application to enantioselective capillary electromigration techniques

Past, present, and future developments in enantioselective analysis using capillary electromigration techniques

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