Journal of separation science最新文献

Molecularly imprinted polymers (MIPs) are very suitable for extraction, drug delivery systems, and sensors due to their good selective adsorption ability, but the difficulty of eluting templates during synthesis and the limitation of application scenarios put higher demands on MIPs. Stimuli-responsive MIPs (SR-MIPs) can actively respond to changes in external conditions to realize various functions, which provides new ideas for the further development of MIPs. This paper reviews the multiple response modes of MIPs, including the common temperature, pH, photo, magnetic, redox-responsive and rare gas, biomolecule, ion, and solvent-responsive MIPs, and explains the mechanism, composition, and applications of such SR-MIPs. These SR-MIPs and the resulting dual/multiple-responsive MIPs have good selectivity, and controllability, and are very promising for isolation and extraction, targeted drug delivery, and electro-sensor.

Sinomenium acutum (Thunb.) Rehd. et Wils is widely used in the treatment of rheumatoid arthritis, with its alkaloid compound sinomenine (SIN) being renowned for its significant anti-inflammatory properties. However, despite its widespread application, the in vivo anti-inflammatory mechanisms and metabolic pathways of SIN remain incompletely understood. This study established a rapid and reliable method based on an ultra-high-performance liquid chromatography method coupled with Quadrupole-Exactive Orbitrap mass spectrometry and molecular docking to identify and characterize SIN and 69 metabolites in rat plasma, urine, and feces, revealing primary metabolic pathways of hydroxylation, demethylation, sulfation, and glucuronidation. Molecular docking results revealed that phase I reactions, including dedimethylation, demethylation, dehydrogenation, and dihydroxylation, along with their composite reactions, were pivotal in influencing SIN's in vivo anti-inflammatory activity. M28, M36, and M59 are potentially the most anti-inflammatory active metabolites of SIN in vivo. This comprehensive analysis unveils SIN's metabolic pathways, offering insights into its biological processes and suggesting a novel approach for exploring active drug constituents. These findings pave the way for further understanding SIN's anti-inflammatory mechanisms, contributing significantly to the development of new therapeutic strategies.

The increasing awareness of environmental issues and the transition to green analytical chemistry (GAC) have gained popularity among academia and industry in recent years. One of the principles of GAC is the reduction and replacement of toxic solvents with more sustainable and environmentally friendly ones. This review gives an overview of the advances in applying green solvents as an alternative to the traditional organic solvents for peptide and protein purification and analysis by liquid chromatography (LC) and capillary electrophoresis (CE) methods. The feasibility of using greener LC and CE methods is demonstrated through several application examples; however, there is still plenty of room for new developments to fully realize their potential and to address existing challenges. Thanks to the tunable properties of designer solvents, such as ionic liquids and deep eutectic solvents, and almost infinite possible mixtures of components for their production, it is possible that some new designer solvents could potentially surpass the traditional harmful solvents in the future. Therefore, future research should focus mainly on developing new solvent combinations and enhancing analytical instruments to be able to effectively work with green solvents.

A dispersive liquid-liquid microextraction based on hydrophobic deep eutectic solvent (hDES) was developed for the extraction and quantification of four cinnamic acid derivatives in traditional Chinese medicines coupled with high-performance liquid chromatography-ultraviolet detection. In this method, a hDES (tetrabutylammonium chloride-hexanoic acid, molar ratio of 1:2) was prepared as the extractant. It only took 15 s to handle multiple samples simultaneously by hand-assisted dispersion. The use of a narrow-bore tube reduced the amount of the hydrophobic extractant with easier recovery. The approach was influenced by several key parameters, including the composition and consumption of the DES, sample phase pH, salt amount, extraction time, and centrifugation time, all of which had been investigated and optimized. Moreover, the formation of the DES was characterized by Fourier-transform infrared spectroscopy and differential scanning calorimetry. Under the optimal conditions, enrichment factors of the target analytes ranged from 135 to 220. Satisfactory linearities (r ≥ 0.9977), detection limits (0.2–0.4 ng/mL), precision (<8.5%), and accuracy (recoveries: 90.0%–104.6%) were obtained. The method has been successfully applied to the simultaneous extraction and preconcentration of four cinnamic acid derivatives in Chinese medicinal samples with rapidness, high efficiency, and convenience.

Sijunzi decoction (SJZD) has been widely used to treat splenic deficiency syndrome. Previous studies confirmed that polysaccharides and non-polysaccharides (NPS) are the main active components of SJZD. This study aimed to investigate the composition and activity of oligosaccharides in NPS. In this study, the oligosaccharide component (named SJZD-OGS), consisting of several different oligosaccharides, was separated and purified from non-polysaccharides of SJZD (SJZD_NPS). Ultra-high-performance liquid chromatography–ion mobility spectrometry–quadrupole time-of-flight mass spectrometry (UHPLC–IMS–QTOF/MS), matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS), and high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD) were used to analyze SJZD-OGS. SJZD-OGS, with a molecular weight of 2178 Da, was composed of glucose and fructose, and its chemical composition mainly included fructo-oligosaccharides (FOS) with a degree of polymerization of 3–14 (DP 3–14). The results of oligosaccharide source exploration demonstrated that the chemical composition of SJZD-OGS was different from that of the oligosaccharides of each herb in SJZD. In addition, SJZD-OGS showed good anti-inflammatory activity on macrophage cells and intestinal epithelial cell protective activity. The present work provides experimental evidence for elucidating the pharmaceutical components of SJZD and presents an effective strategy for the research of oligosaccharides in traditional Chinese medicine (TCM).

The high hydrophobicity and chemical inertness of poly(styrene-divinylbenzene) (PS-DVB) microspheres make their surface hydrophilic modification difficult. Here we describe a facile way to convert PS-DVB microspheres to hydrophilic, then can be used as polar stationary phase for hydrophilic interaction chromatography. This approach utilizes the grafting of an acrylamide-terminated lysine zwitterionic monomer onto PS-DVB microspheres via free radical polymerization. The obtained stationary phase shows good hydrophilicity and a typical retention mechanism of hydrophilic interaction chromatography toward several model polar analytes. It also exhibits obvious zwitterionic properties and is capable of separating cationic and anionic analytes simultaneously. The column shows negligible bleeding level, much superior to silica-based ones.

Recombinant proteins hold significant importance in numerous disciplines. As the demand for expressing and purifying these proteins grows, the scientific community is in dire need of a simple yet versatile methodology that can efficiently purify these proteins. Aptamers as synthetic nucleic acid–based ligands with high affinity have shown promise in this regard, as they can capture targets through molecular recognition. In this study, novel aptamer-functionalized polydopamine-coated magnetic graphene oxide nanocomposites were facilely prepared, achieving an impressive average aptamer coverage density (45 nmol/mg). These nanocomposites exhibited a uniform structure and robust magnetic responsiveness. The findings indicated that they possess several advantages, such as rapid adsorption, substantial capacity (171.4 mg/g), and excellent reusability. Notably, due to the inherent properties of nucleic acids, the immobilized aptamer-magnetic beads can be utilized repeatedly with high purification efficiency. Finally, the nanocomposites were further employed to purify His-tagged proteins from actual samples. Remarkably, they were able to selectively and efficiently isolate His-tagged retinoid X receptor alpha protein from complex Escherichia coli lysate. The purified His-tagged retinoid X receptor alpha protein was analyzed using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. This confirmed the efficacy of developed nanocomposites, reinforcing their vast potential for purification of His-tagged recombinant proteins.

A commercially available dielectric barrier discharge ionization (DBDI) source was tested with supercritical fluid chromatography-mass spectrometry (SFC-MS). The compound mixture investigated comprised caffeine, theobromine, theophylline, uracil, testosterone, and pyrene, diluted in methanol. Dynamic response ranges were evaluated with multiple injections at different concentrations. Precision studies demonstrated the robustness and sensitivity of the ionization source across a concentration range of 10–1000 ng/mL. Results from this experiment showed linear regression of 0.99 or greater for all analytes tested over the range with a relative standard deviation (RSD) of less than 10% down to 10 ng/mL for all analytes except theobromine, which had an RSD of less than 10% down to 25 ng/mL. Notably, this study marks the first investigation of sensitivity for coupling a commercial DBDI source with SFC; a limit of detection less than 1 ng/mL was achieved for all compounds. This study demonstrates chromatographic separation by SFC and MS analysis for compounds that ionize poorly using traditional atmospheric pressure ionization, such as polycyclic aromatic hydrocarbons. Combining SFC with the DBDI source opens promising avenues for analyzing compounds that were previously challenging to characterize with standard atmospheric pressure ionization techniques.