J Sep Sci [JOURNAL]
Sun
200 papers
Synthesis and Validation of Dextran-Based Hydrophilic Magnetic Nanomaterials for Glycopeptide Enrichment.
Cheng L, Fu Q, Huang M … +3 more , Ren H, Wang Y, Xu M
J Sep Sci · 2026 May · PMID 42108716 · Publisher ↗
Glycopeptide enrichment is an essential prerequisite in mass spectrometry (MS)-based protein glycosylation studies, due to the low abundance of glycosylated peptides and the high complexity of biological samples, which c...
Glycopeptide enrichment is an essential prerequisite in mass spectrometry (MS)-based protein glycosylation studies, due to the low abundance of glycosylated peptides and the high complexity of biological samples, which contain substantial interference from non-glycosylated metabolites. Current enrichment strategies commonly exploit the polar interactions between glycans and hydrophilic solid-phase materials. Building on existing magnetic-core particles, we developed a series of novel magnetic materials with surfaces functionalized with dextran and amide groups. The magnetic core, composed of polyvinylpyrrolidone (PVP) and FeO, was sequentially coated with SiO and dextran. Amide groups were then conjugated to the dextran layer via a condensation reaction between carboxy-modified dextran and ethanolamine. The glycopeptide enrichment performance of five resulting magnetic materials was evaluated using IgG and rat serum samples. One material, designated FeO@SiO@Dextran-Amide (Dextran-polyamide-717), demonstrated superior sensitivity for glycopeptide detection and strong resistance to nonspecific interference. Moreover, Dextran-polyamide-717 exhibited higher enrichment efficiency in both IgG and serum samples compared to two commercially available products. With its multilayer surface modification strategy, Dextran-polyamide-717 shows great promise for advanced applications in glycoproteomic research.
Ultrasound-Assisted Extraction Coupled With Derivatization for Sensitive High-Performance Liquid Chromatography Determination of Resorcinol in Permanent Hair Dyes.
Ntorkou M, Letsika K, Tzanavaras PD … +1 more , Zacharis CK
J Sep Sci · 2026 May · PMID 42108707 · Full text
Resorcinol is widely used as an oxidative dye intermediate in commercial hair coloring products, yet its accurate quantification remains challenging due to its limited native fluorescence and the strong interferences ass...
Resorcinol is widely used as an oxidative dye intermediate in commercial hair coloring products, yet its accurate quantification remains challenging due to its limited native fluorescence and the strong interferences associated with complex cosmetic matrices. In this study, we report a sensitive and selective high-performance liquid chromatography-fluorescence method based on dopamine derivatization for the trace-level determination of resorcinol in hair dye formulations. The analyte was isolated from the sample matrix using ultrasound-assisted extraction with methanol. Under mild alkaline conditions, dopamine rapidly forms a highly fluorescent adduct with resorcinol, substantially enhancing analytical sensitivity and selectivity. The method was optimized with respect to derivatization parameters, chromatographic separation, and detector response. Validation demonstrated excellent linearity over the range of 1-75 ng/mL (r > 0.999), a low limit of detection (= 0.3 ng/mL), and satisfactory recoveries (76.0%-118.0%) across spiked matrices. The robustness of the derivatization procedure was evaluated using Monte-Carlo simulation experiments. Method greenness was assessed using the multicolor tool, yielding a score of 69.9%. Application to commercial products revealed resorcinol concentrations consistent with reported regulatory limits. The proposed method demonstrates promising potential for routine analytical applications; however, further validation, including inter-laboratory studies and comparison with established reference methods, is required to support its suitability for regulatory use.
Losartan API and Nitrosamines Impurities-Stability Profile Investigation Using HPLC, LC-MS, and In Silico Assessment.
Martini PRR, Machioli LF, Santos BPD … +4 more , Oliveira TF, Paula FR, Paim CS, Mendez ASL
J Sep Sci · 2026 May · PMID 42104572 · Full text
Nitrosamines are potent genotoxic impurities with well reported mutagenic and carcinogenic effects. Their presence has been detected in several pharmaceutical products among them losartan, an angiotensin II receptor bloc...
Nitrosamines are potent genotoxic impurities with well reported mutagenic and carcinogenic effects. Their presence has been detected in several pharmaceutical products among them losartan, an angiotensin II receptor blocker. Considering the risks already reported for these impurities, the present study aimed to investigate the influence of four common nitrosamines-N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosodiisopropylamine (NDIPA), and N-nitrosodibutylamine (NDBA)-in the stability profile of losartan API. Quantitative assay was conducted through HPLC and LC-MS, with focus on monitoring degradation rate and degradation products under influence of nitrosamines. Predictive data by in silico investigation employing Zeneth Nexus and Spartan were simultaneously studied, considering degradation products, fragmentation pathway and nitrosamines reactivity. The drug residual content showed variability depending on the nitrosamine evaluated and the stressing condition applied. From photolysis, for example the residual content ranged 80%-90%, with a greater decomposition in samples containing nitrosamines. A greater decomposition was also observed in oxidative degradation, with exception for samples containing NDMA. Acid and basic media caused a significant decomposition, with the residual losartan content in a range of 41%-52% and 28%-51%, respectively. From LC-MS analyzes, these impurities were mostly not detected in the degraded samples, suggesting their consumption during the reaction due to their reactivity. A protective effect from nitrosamines can be also reported possibly due to their reactivity against the stressing factor. Seven degradation products were structurally proposed by LC-MS at m/z 449, m/z 447, m/z 366, m/z 338, m/z 274, m/z 391, and m/z 341, some of them predicted computationally by Zeneth.
Sample Preparation and Separation of Lignans by Liquid Chromatography.
Paloluoto M, Wiedmer SK
J Sep Sci · 2026 May · PMID 42087627 · Full text
Lignans are important phytochemicals found mostly in the resins of coniferous trees, but are also introduced into human diets through foods such as sesame seeds and extra-virgin olive oil. They are pharmacologically inte...
Lignans are important phytochemicals found mostly in the resins of coniferous trees, but are also introduced into human diets through foods such as sesame seeds and extra-virgin olive oil. They are pharmacologically interesting mainly because of their antioxidant activities, and they have also been shown to have cytotoxic and antimicrobial effects. Lignans are typically analyzed using liquid chromatography, although the complexity of the common matrices from which lignans are studied requires extensive sample preparation methodologies beforehand. While the simplest samples, such as wines and olive oils, can be analyzed without complicated procedures, most samples will require purification through liquid‒liquid extraction or silica gel column chromatography. Lignans are most often detected using mass spectrometry or ultraviolet‒visible spectrophotometry, but other methods, such as fluorescence and coulometric electrode array detectors, have also been proven useful. In this review, we will describe the typical characteristics of lignans with focus on their main pharmaceutical benefits, as well as typical sample preparation methodologies and liquid chromatographic analyses.
Semi-Quantitative Determination of Volatile Organic Compounds Detected in Air Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry.
Karimkyzy N, Bukenov B, Bakaikina NV … +3 more , Kurmanbayeva T, Dyussenkulova B, Kenessov B
J Sep Sci · 2026 May · PMID 42087624 · Publisher ↗
Nontargeted air analysis using methods based on gas chromatography (GC) and mass spectrometry (MS) is very important for the discovery of new potentially dangerous volatile organic compounds (VOCs). Solid-phase microextr...
Nontargeted air analysis using methods based on gas chromatography (GC) and mass spectrometry (MS) is very important for the discovery of new potentially dangerous volatile organic compounds (VOCs). Solid-phase microextraction (SPME) is one of the simplest and cost-efficient sampling techniques for screening VOCs in air, but the extraction effectiveness of detected compounds can substantially vary depending on their properties and affinity to the fiber coating. This study was aimed at the development of a novel method for semi-quantitative determination of VOCs identified in air samples using SPME and GC-MS. Extraction effectiveness was estimated from fiber coating-air distribution constants predicted using linear solvation energy relationship and numerical modeling with COMSOL Multiphysics. MS detector response factors were estimated using multiple regression obtained from experimental responses of 111 VOCs and SVOCs, their molecular weights, octanol-water partitioning coefficients, polar surface areas, and fractional ion abundances of base ions. Numerical modeling using COMSOL Multiphysics improved the accuracy for less volatile analytes with greater molecular weight, particularly at lower extraction times. For 12 of 14 tested analytes, recoveries from spiked nitrogen samples were in the range between 39% and 275%. The developed method was successfully applied for determining approximate concentrations of VOCs identified in samples of air, and for determination of approximate time-weighted average concentrations of VOCs. It can be recommended for the quick estimation of approximate concentrations of VOCs detected during nontargeted analysis when calibration standards are not available or when high accuracy is not needed.
Replacing Ecologically Risky Trifluoroacetic Acid and Acetonitrile With Methanesulfonic Acid and Dimethyl Carbonate in High-Performance Liquid Chromatography Analyses of Small Molecule Drugs.
Steinicke FPN, El-Jourani TB, Haegner J … +2 more , Schiedel M, Wätzig H
J Sep Sci · 2026 May · PMID 42087586 · Full text
It has long been recognised that, in the long term, hazardous acetonitrile (ACN) as a mobile-phase component and the environmentally critical trifluoroacetic acid (TFA) as an ion-pairing reagent should be replaced in hig...
It has long been recognised that, in the long term, hazardous acetonitrile (ACN) as a mobile-phase component and the environmentally critical trifluoroacetic acid (TFA) as an ion-pairing reagent should be replaced in high-performance liquid chromatography (HPLC). Nevertheless, methods relying on precisely these reagents are still widely used. Herein, we show that alternative approaches for the analysis of small molecule drugs are readily applicable, using examples from pharmaceutical quality control and medicinal chemistry. First, the principles of green analytical chemistry were implemented in an alternative HPLC method for the theophylline monohydrate monograph of the European Pharmacopoeia, without altering the core methodology. Among the various conditions tested, the use of 2% dimethyl carbonate (DMC) provided equivalent separation and an even slightly improved resolution compared with the original ACN-based pharmacopoeial method. In a second approach, we present a highly sustainable gradient HPLC method for routine purity analysis of synthesis products by replacing TFA with safe, biodegradable, and environmentally benign methanesulfonic acid (MSA). Furthermore, in the case of this gradient method, ACN could be replaced by the biodegradable and environmentally friendly DMC. An eluent composition consisting of 42 parts DMC, 23 parts EtOH, 35 parts HO and 0.1 parts MSA was found to be equivalent to ACN containing 0.1% TFA. By employing a reproducible protocol using EtOH as a co-solvent, we were able to overcome current challenges associated with the use of organic carbonates in HPLC, which primarily arise from their limited miscibility with water. Given the continued widespread use of gradient HPLC methods employing ACN as an eluent and TFA as an acidic modifier, the methods presented herein offer significant potential to advance the implementation of sustainability in pharmaceutical quality control and medicinal chemistry.
Homochiral Metal-organic Framework (+)-diacetyl-L-tartaric-NH-MIL-101(Fe) as Stationary Phase for Enantioseparation in Capillary Electrochromatography.
Yu J, Guan J, Long K … +3 more , Chen X, Shi S, Jiang X
J Sep Sci · 2026 May · PMID 42087578 · Publisher ↗
A novel enantioselective open-tubular capillary electrochromatography (CEC) column was fabricated by noncovalently immobilizing (+)-diacetyl-L-tartaric anhydride functionalized NH-MIL-101(Fe) onto the capillary inner wal...
A novel enantioselective open-tubular capillary electrochromatography (CEC) column was fabricated by noncovalently immobilizing (+)-diacetyl-L-tartaric anhydride functionalized NH-MIL-101(Fe) onto the capillary inner wall using polydopamine as an adhesive layer. The coating of the modified capillary was comprehensively characterized through Fourier-transform infrared spectroscopy, powder X-ray diffraction, Brunauer-Emmett-Teller analysis, scanning electron microscopy, energy dispersive X-ray spectroscopy, circular dichroism, and electroosmotic flow measurements. The column's chiral separation ability was assessed by analyzing seven model compounds, comprising four proton pump inhibitors (omeprazole, pantoprazole, lansoprazole, and tenatoprazole) and three fluoroquinolones (ofloxacin, sparfloxacin, and gatifloxacin). Under optimized conditions, baseline resolution (9.68-14.56) of all enantiomers was achieved within 7 min. The column demonstrated excellent reproducibility, with inter-day, intra-day, and column-to-column relative standard deviations ranging from 1.22% to 4.98%. Additionally, molecular docking simulations were conducted using AutoDock Tools to investigate interactions between the stationary phase and analyte enantiomers, with computational results corroborating experimental CEC data.
Multistep Plunger Injection Assisted Micellar-to-Solvent Stacking for the Determination of Alkaloids From Medicinal Plants Using Capillary Zone Electrophoresis.
Fan KY, Jin QZ, Niu SQ … +2 more , Cao J, Ye LH
J Sep Sci · 2026 May · PMID 42083389 · Publisher ↗
A simple, rapid, and efficient multistep plunger injection-assisted micellar to solvent stacking method was developed for the determination of cationic analytes from medicinal plants. In this method, a three-step sequent...
A simple, rapid, and efficient multistep plunger injection-assisted micellar to solvent stacking method was developed for the determination of cationic analytes from medicinal plants. In this method, a three-step sequential injection protocol was used, where sodium dodecyl sulfate (SDS), sample, and methanol (MeOH) solutions were introduced in succession to achieve an effective enrichment. The background solution contained 30 mM sodium dihydrogen phosphate and 30 mM citric acid. To achieve optimal enrichment efficiency, we systematically optimized several key parameters: surfactant type, SDS concentration, sodium dihydrogen phosphate concentration in the sample matrix, MeOH concentration, SDS injection time, MeOH injection time, and sample injection time. The optimal stacking conditions were as follows: injection of 10 mM SDS for 30 s, injection of the sample solution for 60 s, and injection of 40% MeOH for 10 s. This method exhibited an excellent linear relationship, as evidenced by the correlation coefficients (R) ranging from 0.994 to 0.999. The intra-day and inter-day precision of this method was less than 3.701%, and the recovery rates of the analytes ranged from 92.70% to 107.79%, indicating satisfactory accuracy and reliability. Compared with conventional injection techniques, the sensitivity enrichment factors of the four analytes ranged from 42 to 44. The proposed method was validated for its applicability in detecting four alkaloids (fumarine, allocryptopine, tetrahydropalmatine, and corydaline) in Rhizoma corydalis samples.
Hydrophobic Menthol-Based Deep Eutectic Solvent for Ultrasound-Assisted Dispersive Liquid‒Liquid Microextraction of Amide Herbicides in Food and Environmental Samples Before Determination by HPLC.
Xie M, Huang G, Wang H … +4 more , Wei J, Lin J, Huang Y, Ruan G
J Sep Sci · 2026 May · PMID 42083338 · Publisher ↗
Toxic amide herbicide residues pose significant risks to food safety and environmental health. In this study, an ultrasound-assisted dispersive liquid‒liquid extraction method utilizing a hydrophobic menthol-based deep e...
Toxic amide herbicide residues pose significant risks to food safety and environmental health. In this study, an ultrasound-assisted dispersive liquid‒liquid extraction method utilizing a hydrophobic menthol-based deep eutectic solvent (DES) was developed for the efficient separation and determination of four amide herbicides in complex matrices, including vegetables, soil, and water. DES composed of decanoic acid (hydrogen bond acceptor) and menthol (hydrogen bond donor) at a molar ratio of 2:3 demonstrated superior extraction performance compared to those using lauric or oleic acid as a hydrogen bond acceptor. The extraction was equilibrated within 2 min under neutral pH conditions. Molecular docking simulations revealed that the N─H groups in the amide moieties served as the primary active sites for hydrogen bonding interactions with the DES. By integrating this green extraction technique with high-performance liquid chromatography, a robust analytical method was established, exhibiting excellent linearity (R > 0.9991) over a wide range (1-200 ng mL), with low limits of detection (0.3-0.5 ng mL) and high precision (intraday RSDs ≤ 3.6%, inter-day RSDs ≤ 8.2%). The method achieved high recoveries (89.8%-116%) across various samples. Greenness assessments using the GAREEprep and Analytical Ecological Scale showed scores of 0.57 and 85, respectively, underscoring the sustainability of the method. This study presents a rapid, sensitive, and sustainable alternative for monitoring amide herbicide residues, contributing to food safety and environmental protection.
From Columns to Clouds: Emerging Interfaces and Ion Sources for Coupling Analytical Separations With Mass Spectrometry.
Raju CM, Urban PL
J Sep Sci · 2026 May · PMID 42080417 · Publisher ↗
Although mass spectrometry (MS) is a powerful analytical technique, it is vulnerable to matrix interference, and it does not distinguish ions with the same m/z (isobaric interference). Therefore, for the past few decades...
Although mass spectrometry (MS) is a powerful analytical technique, it is vulnerable to matrix interference, and it does not distinguish ions with the same m/z (isobaric interference). Therefore, for the past few decades, numerous efforts have been made to enable coupling separation systems with MS. Apart from a set of mainstream hyphenation approaches (such as those using inductively coupled plasma ionization, electron ionization, and electrospray ionization), a number of less conventional ways to couple separation systems with MS have been devised. Extraordinary methods for coupling gas chromatography, liquid chromatography, capillary electrophoresis, thin-layer chromatography, supercritical fluid chromatography, and other unconventional interfaces and ion sources have been disclosed in the literature. Some of these techniques extend the analyte coverage of traditional hyphenated techniques by enabling the detection of less polar compounds. Others speed up analysis or decrease the cost. Another notable trend is the implementation of the so-called ambient ionization techniques for coupling separations with MS.
Design of Experiments-assisted Micellar Electrokinetic Chromatography Separation of Phosphodiesterase-5 Inhibitors: Application to Sildenafil and Tadalafil.
Niculaș C, Hancu G, Szabó ZI … +3 more , Gabriela Cârje A, Ion V, Muntean DL
J Sep Sci · 2026 May · PMID 42068125 · Publisher ↗
A micellar electrokinetic chromatography method was developed for the simultaneous separation of the phosphodiesterase-5 inhibitors sildenafil and tadalafil, two therapeutic agents used in the treatment of erectile dysfu...
A micellar electrokinetic chromatography method was developed for the simultaneous separation of the phosphodiesterase-5 inhibitors sildenafil and tadalafil, two therapeutic agents used in the treatment of erectile dysfunction that are frequently identified as illicit adulterants in dietary supplements marketed for sexual enhancement. Method development was supported by a design of experiments strategy. An initial fractional factorial screening design was used to evaluate the influence of selected experimental parameters on resolution (R) and migration time. Pareto analysis of standardized effects indicated that cyclodextrin (CD) concentration, methanol (MeOH) content, and separation voltage significantly affected the separation, whereas pH, sodium dodecyl sulfate (SDS) concentration, and temperature did not show a statistically significant impact within the studied range. Based on the screening results, a Box-Behnken response surface design was employed to optimize the significant factors. Optimized separation conditions consisted of a 50 mM phosphate buffer (pH 2.5) containing 50 mM SDS, 10% MeOH, and 5 mM hydroxypropyl-β-CD, with a separation voltage of -20 kV and a capillary temperature of 20°C. Under these conditions, baseline separation was achieved with a R of 4.75 and migration times below 6 min. The method was validated in terms of precision, linearity, accuracy, and robustness, showing satisfactory analytical performance. Application to pharmaceutical formulations and dietary supplement samples confirmed the suitability of the proposed method for routine screening and quality control purposes.
A Monoclonal Antibody-based Lateral Flow Immunochromatographic Assay for Rapid Detection of Derrisisoflavone A in Derris scandens (Roxb.) Benth.
Srimongkon P, Sae-Foo W, Yusakul G … +1 more , Putalun W
J Sep Sci · 2026 May · PMID 42068121 · Publisher ↗
Derrisisoflavone A is a prenylated isoflavonoid and a chemical marker in the stem of Derris scandens (Roxb.) Benth., it is a suitable chemical marker for this plant. Conventional analytical techniques, such as high-perfo...
Derrisisoflavone A is a prenylated isoflavonoid and a chemical marker in the stem of Derris scandens (Roxb.) Benth., it is a suitable chemical marker for this plant. Conventional analytical techniques, such as high-performance liquid chromatography, liquid chromatography-mass spectrometry, and immunoassays, offer high sensitivity but rely on complex analytical equipment and specialized expertise, thereby limiting their applicability for rapid on-site analysis. In this study, a lateral flow immunochromatographic assay (LFIA) employing gold nanoparticle (AuNP)-labeled monoclonal antibodies (mAbs) was developed for qualitative detection of derrisisoflavone A in D. scandens plant materials and herbal products. The LFIA was designed in a competitive format using AuNPs-mAbs conjugates as the detection probe, derrisisoflavone A-cationized ovalbumin conjugates applied on the test zone, and anti-mouse immunoglobulin G antibody on the control zone. Under optimized conditions, the assay was evaluated for sensitivity and specificity and validated by comparison with a well-established indirect competitive enzyme-linked immunosorbent assay (icELISA) using various D. scandens plant parts, commercial products, and representative Fabaceae species. The LFIA exhibited a visual limit of detection of 100 µg/mL, defined by complete inhibition of the test zone signal, and demonstrated high analytical specificity with undetectable cross-reactivity toward structurally related isoflavonoids or prenylated flavonoids. The analytical results showed good agreement with those obtained by icELISA. Although less sensitive than quantitative methods, the developed LFIA provides a rapid, simple, and reliable screening tool for on-site quality control and preliminary assessment of derrisisoflavone A in D. scandens and related products.
Development and Validation of a Sensitive UHPLC-MS/MS Method for the Simultaneous Determination of 19 Bile Acids in Liver and Feces: Application to Metabolic Dysfunction-Associated Steatotic Liver Disease Mice.
Xiao M, Zhao W, Ba Y … +6 more , Xia M, Luo K, You L, Li X, Zan K, Chen X
J Sep Sci · 2026 May · PMID 42068119 · Publisher ↗
Recently, bile acids (BAs) have garnered significant attention due to their crucial roles in various metabolic diseases. However, the simultaneous quantification of BAs in biological samples is challenging due to the str...
Recently, bile acids (BAs) have garnered significant attention due to their crucial roles in various metabolic diseases. However, the simultaneous quantification of BAs in biological samples is challenging due to the structural similarities, complex biological matrix, and tissue-specific distribution. We developed a sensitive UHPLC-MS/MS method for quantitation of 19 BAs in mouse liver (mainly conjugated BAs) and feces (mainly unconjugated BAs). We compared protein precipitation, liquid-liquid extraction, and solid-phase extraction (SPE) methods for sample preparation, and SPE was chosen due to the low background noise and high extraction efficiency for both conjugated and unconjugated BAs. The method was extensively validated by evaluating the linearity (R ≥ 0.991), extraction recovery (82%-112%), limits of detection (1-2 ng/mL) and low limits of quantification (2-5 ng/mL). Then, the method was applied to the detection of BAs in liver and feces of metabolic dysfunction-associated steatotic liver disease mice, and the correlations between BA levels and the mRNA expression levels of BA metabolic enzymes, transporters, and receptors were analyzed. This study provides a direct and reliable determination method for the in-depth investigation of the enterohepatic circulation of BAs.
Correction to "Comparative Chromatographic Separation of Free Radicals from Natural Products Using Green Organic Solvents".
J Sep Sci · 2026 Apr · PMID 42047001 · Publisher ↗
Abstract loading — click title to view on PubMed.
Identification and Quantification of Isomeric Disaccharides From Honey and Beer Using Trapped Ion Mobility Spectrometry.
Cai Y, Jiang B, Wang B … +3 more , Meng L, Yan Y, Cai T
J Sep Sci · 2026 Apr · PMID 42046904 · Publisher ↗
The specific discrimination of carbohydrate structures is crucial for understanding their critical roles in biological functions and effects. Distinguishing multiple isomers in monosaccharide composition, types of isomer...
The specific discrimination of carbohydrate structures is crucial for understanding their critical roles in biological functions and effects. Distinguishing multiple isomers in monosaccharide composition, types of isomeric configurations, and glycosidic linkages remains a challenge. This study presents a method for the identification and quantification of disaccharide isomers based on the distinct structural or shape differences of complexes formed between disaccharides and metal ions (Na, K, Rb, Cs, and Mg), or between disaccharides and cyclodextrins (α, β, and γ), as analyzed by trapped ion mobility spectrometry-mass spectrometry (TIMS-MS). Additionally, the method was utilized for the analysis of real samples including honey and beer, enabling the targeted extraction, identification, and quantification of disaccharide isomers. Quantitative curves were conducted to validate the quantitative ability of the method to distinguish maltose, lactose, and sucrose isomers. This simple, cost-effective strategy has broad potential applications for the analysis of disaccharide isomers in the food industry, as well as for the geographical origin traceability of foods containing disaccharides.
Green and Efficient Extraction of Polyphenols From Lonicera caerulea L. Berries and Evaluation of Their Antioxidant and Lipid-Lowering Activities.
Feng P, Gui Q, Yi J … +7 more , Zhang W, Feng Y, Tao J, Wang F, Wu J, Kawagishi H, Wang P
J Sep Sci · 2026 Apr · PMID 42032917 · Publisher ↗
The demand for sustainable methods to extract bioactive compounds from fruits is increasing, yet conventional extraction methods are limited by their reliance on large amounts of organic solvents, limiting their widespre...
The demand for sustainable methods to extract bioactive compounds from fruits is increasing, yet conventional extraction methods are limited by their reliance on large amounts of organic solvents, limiting their widespread application. Therefore, we evaluated a deep eutectic solvent (DES)-ultrasound-assisted extraction to efficiently extract phenolic compounds from Lonicera caerulea L. berries. Using single-factor experiments and response surface methodology, the optimal conditions were determined: A DES composed of choline chloride and 1,3-butanediol at a 1:5 molar ratio, with 29% water content, a solid-liquid ratio of 1:41 g/mL, and ultrasonication for 50 min. This method yielded 68.63 ± 0.46 mg gallic acid/g of total polyphenols, a 1.5-fold increase over the conventional solvent (50% ethanol). Furthermore, UHPLC-Q-TOF-MS/MS analysis confirmed the presence of 31 phytochemicals in the extract, including cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside, chlorogenic acid, procyanidin B2, rutin, and quercitrin, among others. Scanning electron microscopy analysis confirmed the synergistic mechanism of DES permeation and ultrasound-induced cell wall disruption, and the mechanism of DES formation was studied by Fourier transform infrared spectroscopy. Further studies revealed that the extract exhibited significant antioxidant activity, with IC values of 8.57 ± 0.19 µg/mL, 409.13 ± 6.77 µg/mL, and 123.17 ± 3.25 µg/mL for DPPH•, •OH, and ABTS• assays, respectively, and demonstrated pancreatic lipase inhibition with an IC of 4.31 ± 0.12 mg/mL. In the zebrafish model of non-alcoholic fatty liver disease, the extract (200 µg/mL) significantly reduced hepatic lipid accumulation, and decreased total cholesterol, triglycerides, alanine aminotransferase, and aspartate aminotransferase levels by 64%, 60%, 60%, and 55%, respectively, confirming potent lipid-lowering and hepatoprotective efficacy. Overall, DES combined with ultrasound-assisted extraction could serve as an eco-friendly method for recovering high-value compounds from fruits and their byproducts.
An Accurate Method Based on Ultra-High-Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry for the Quantification of Five Cannabinoids in Juvenile and Adult Caenorhabditis elegans.
Sepehr E, Zhao Y, Vaught CA … +5 more , Camacho JA, Welch B, Yourick J, Sprando RL, Hunt PR
J Sep Sci · 2026 Apr · PMID 42024230 · Full text
Caenorhabditis elegans is an alternative model organism for toxicology research that aligns with the 3Rs principle (Replace, Reduce, Refine) and new approaches to modernize toxicity testing strategies. This study develop...
Caenorhabditis elegans is an alternative model organism for toxicology research that aligns with the 3Rs principle (Replace, Reduce, Refine) and new approaches to modernize toxicity testing strategies. This study developed and single-laboratory validated a sensitive ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UHPLC-ESI-MS/MS) method for quantifying five cannabinoids- cannabidivarin, cannabigerol, cannabidiol, cannabinol, and cannabichromene- in juvenile and adult C. elegans matrices. Homogenized C. elegans samples were spiked with labeled internal standards and subjected to protein precipitation. The resulting supernatants were injected onto a Waters ACQUITY UPLC BEH C18 column (130 Å, 1.7 µm, 2.1 × 100 mm), coupled to an Agilent 6460 Triple Quadrupole mass spectrometer detector, allowing for the detection and quantification of target analytes in a total run time of 14 min using a 50 µL sample volume. Single-laboratory method validation was performed using spiked quality control samples, consisting of six replicates at four concentrations of all cannabinoids in juvenile and adult C. elegans matrices, analyzed over three consecutive days. The validated method demonstrated linear regression calibration curves with R ≥ 0.99 across the concentration range of 0.1-7.5 µg/mL for all cannabinoids. The intra-day accuracy in juvenile and adult C. elegans was within 85-108% and 97-109% of the fortified concentration, respectively, with intra-day precision between 1.28-4.62% relative standard deviation (RSD) and 0.64-5.60% RSD. Similarly, the inter-day accuracy was within 86-110% and 97-106% of the fortified concentration, respectively, with the inter-day precision between 2.06-5.62% RSD and 1.42-10.9% RSD. This single laboratory validated UHPLC-ESI-MS/MS method provides accurate and reliable cannabinoid quantification and facilitates the translational utility of cannabinoid toxicity testing in C. elegans. Analytical method development to accurately detect chemicals within diverse tissue matrices supports dosimetry and toxicokinetic analyses, essential steps toward investigating food chemical safety.
Heart-Cutting Two-Dimensional Liquid Chromatography-Isotope Ratio Mass Spectrometry for Compound-Specific δC Analysis of Water-Soluble B Vitamins in Complex Supplement Matrices.
Rockel SP, Martiny J, Jochmann MA … +1 more , Schmidt TC
J Sep Sci · 2026 Apr · PMID 42013051 · Full text
Compound-specific stable carbon isotope analysis by one-dimensional liquid chromatography-isotope ratio mass spectrometry (LC-IRMS) is fundamentally constrained by the requirement for fully aqueous mobile phases, which l...
Compound-specific stable carbon isotope analysis by one-dimensional liquid chromatography-isotope ratio mass spectrometry (LC-IRMS) is fundamentally constrained by the requirement for fully aqueous mobile phases, which limits chromatographic selectivity and prevents effective separation of analytes from complex sample matrices. Here, a heart-cutting two-dimensional LC-IRMS method (2D-LC-IRMS) is presented for the first compound-specific δC analysis of the water-soluble vitamins B5 (pantothenic acid) and B9 (folic acid) in commercial dietary supplements and fortified beverages. An organic-modified reversed-phase separation in the first dimension achieved matrix reduction, while a fully aqueous second-dimension separation ensured IRMS compatibility and delivered baseline-resolved analyte peaks for precise isotope determination. Validation demonstrated linear calibration over 2-100 mgC L with R ≥ 0.9999, repeatability of ≤ 0.13‰, and isotope-stability-based method detection limits of 5 mgC L. Analyzed δC values were independent of chromatographic configuration, confirming that heart-cutting transfer does not introduce isotope fractionation. Application to 12 commercial products, including tablets, effervescent formulations, powdered supplements, and an energy drink, yielded δC ranges of -20.6‰ to -32.9‰ for vitamin B5 and -20.4‰ to -36.4‰ for vitamin B9, reflecting differences in synthetic production routes across manufacturers. The presented workflow extends LC-IRMS to the compound class of water soluble vitamins that were so far inaccessible to this technique and provides a broadly applicable strategy for compound-specific isotope analysis of polar analytes in challenging matrices.
Study on the Mechanism of Component Evolution and Viscosity Change Based on Temperature Differences in In-Situ Combustion of Paraffinic Heavy Oil.
Guo F, Chen H, Li Y … +4 more , Zeng Q, Guo Y, Liang X, Wang X
J Sep Sci · 2026 Apr · PMID 42013050 · Publisher ↗
This study investigated the relationship between component evolution and viscosity reduction in the Menggulin paraffinic crude oil reservoir under reservoir conditions using gas chromatography-mass spectrometry and visco...
This study investigated the relationship between component evolution and viscosity reduction in the Menggulin paraffinic crude oil reservoir under reservoir conditions using gas chromatography-mass spectrometry and viscosity measurements at reservoir temperature (37.2°C). Results show stage-dependent compositional transformation: in 250-400°C medium-temperature oxidation, C-C components are fully combusted, with displaced oil dominated by residual alkanes and oxygenates, yielding limited viscosity reduction. Above 400°C (high-temperature cracking), long-chain n-alkanes undergo β-scission to generate abundant C-C+ long-chain α-olefins, which reduce viscosity via physical dilution and polar interaction with wax crystals/resins. Specifically, 10% addition of 500°C-displaced oil lowers the original 853 mPa·s viscosity to ∼200 mPa·s (88% reduction), outperforming 250°C-displaced oil (needing >25% addition). This study reveals that Menggulin crude exhibits a unique olefin-dominated evolution, identifies long-chain α-olefins as the signature products of paraffinic crude during in-situ combustion (ISC), verifies temperatures above 400°C as the optimal temperature window, and thus provides a scientific basis for the optimization of ISC in similar reservoirs.
Residual Status of 25 Veterinary Drugs and Dietary Exposure Assessment of Commercially Available Pork in Guiyang.
Liu D, Yang J, Cao L … +5 more , Li Z, Ji T, Tang D, Song X, Ou D
J Sep Sci · 2026 Apr · PMID 42013011 · Publisher ↗
Intensive farming practices have necessitated the extensive use of veterinary drugs, raising significant concerns regarding residue contamination. Consequently, long-term monitoring of residues and the evaluation of diet...
Intensive farming practices have necessitated the extensive use of veterinary drugs, raising significant concerns regarding residue contamination. Consequently, long-term monitoring of residues and the evaluation of dietary exposure risks are essential. In this study, 326 pork samples were collected from local supermarkets between October 2024 and April 2025. Methods were developed for the analysis of 25 veterinary drugs (including sulfonamides, tetracyclines, fluoroquinolones, β-agonists, amphenicols, macrolides, and roxarsone) using high-performance liquid chromatography-tandem mass spectrometry. Roxarsone was extracted using a methanol/water solution (6:4, v/v), and amphenicols were extracted with a 2% ammonia in ethyl acetate solution. Other analytes were extracted with acetonitrile containing 2% acetic acid, followed by cleanup via dispersive solid-phase extraction. Chromatographic separation and detection were performed under multiple reaction monitoring conditions in both positive and negative ionization modes. The method exhibited good linearity (r > 0.99) for all target analytes. Recoveries ranged from 70% to 110% with relative standard deviations below 13%, and limits of quantitation ranged from 0.02 to 5.0 µg/kg. Tetracyclines were the most frequently detected class (detection rate of 63.6%), whereas prohibited substances (β-agonists and roxarsone) were not detected. Residue levels exhibited seasonal fluctuations, with tetracyclines peaking in October and fluoroquinolones and amphenicols in November. Hazard quotient values for dietary intake were consistently below 1, indicating a low health risk to consumers. The dynamic monitoring of drug residue levels offers a more comprehensive approach compared to static methods, which provides valuable insights to guide the rational use of veterinary drugs.
About
- Frequency
- Sun
- Papers found
- 200
- RSS feed
- Subscribe