Developing a chiral material as versatile and universal chiral stationary phase(CSP) for chiral separation in diverse chromatographic techniques simultaneously is of great significance.In this study,we demonstrated fo...Developing a chiral material as versatile and universal chiral stationary phase(CSP) for chiral separation in diverse chromatographic techniques simultaneously is of great significance.In this study,we demonstrated for the first time that a chiral metal-organic cage(MOC),[Zn_(6)M_(4)],as a universal chiral recognition material for both multi-mode high-performance liquid chromatography(HPLC) and capillary gas chromatography(GC) enantioseparation.Two novel HPLC CSPs with different bonding arms(CSP-A with a cationic imidazolium bonding arm and CSP-B with an alkyl chain bonding arm) were prepared by clicking of functionalized chiral MOC [Zn_(6)M_(4)] onto thiolated silica via thiol-ene click chemistry.Meanwhile,a capillary GC column statically coated with the chiral MOC [Zn_(6)M_(4)] was also fabricated.The results showed that the chiral MOC exhibits excellent enantioselectivity not only in normal phase HPLC(NP-HPLC) and reversed phase(RP-HPLC) but also in GC,and various racemates were well separated,including alcohols,diols,esters,ketones,ethers,amines,and epoxides.Importantly,CSP-A and CSP-B are complementary to commercially available Chiralcel OD-H and Chiralpak AD-H columns in enantioseparation,which can separate some racemates that could not be or could not well be separated by the two widely used commercial columns,suggesting the great potential of the two prepared CSPs in enantioseparation.This work reveals that the chiral MOC is potential versatile chiral recognition materials for both HPLC and GC,and also paves the way to expand the potential applications of MOCs.展开更多
Metal organic framework(MOF) assembled with coordination bonds has the disadvantage of poor stability that limits its application in the field of stationary phase,while covalent organic framework(COF)assembled through...Metal organic framework(MOF) assembled with coordination bonds has the disadvantage of poor stability that limits its application in the field of stationary phase,while covalent organic framework(COF)assembled through covalent bonds exhibits excellent structural stability.It has been shown that the stationary phases prepared by combining MOF and COF can make up for the poor stability of MOF@SiO_(2),and the MOF/COF composites have superior chromatographic separation performance.However,the traditional methods for preparing COF/MOF based stationary phases are generally solvent thermal synthesis.In this study,a green and low-cost synthesis method was proposed for the preparation of MOF/COF@SiO_(2) stationary phase.Firstly,COF@SiO_(2) was prepared in a choline chloride/ethylene glycol based deep eutectic solvent(DES).Secondly,another acid-base tunable DES prepared by mixing p-toluenesulfonic acid(PTSA)and 2-methylimidazole in different proportions was introduced as the reaction solvent and reactant for rapid synthesis of MOF/COF@SiO_(2).Compared with the toxic transition metal-based MOFs selected in most previous studies,a lightweight and non-toxic S-zone metal(calcium) based MOF was employed in this study.PTSA and calcium will form the calcium/oxygen-containing organic acid framework in acidic DES,which assembles with terephthalic acid dissolved in basic DES to form MOF.The strong hydrogen bonding effect of DES can facilitate rapid assembly of Ca-MOF.The obtained Ca-MOF/COF@SiO_(2) can be used for multi-mode chromatography to efficiently separate multiple isomeric/hydrophilic/hydrophobic analytes.The synthesis method of Ca-MOF/COF@SiO_(2) is green and mild,especially the use of acid-base tunable DES promotes the rapid synthesis of non-toxic Ca-MOF/COF@silica composites,which offers an innovative approach of greenly synthesizing novel MOF/COF stationary phases and extends their applications in the field of chromatography.展开更多
Arsenic speciation in freshwater fish is crucial for providing meaningful consumption guidelines that allow the public to make informed decisions regarding its consumption.While marine fish have attractedmuch research...Arsenic speciation in freshwater fish is crucial for providing meaningful consumption guidelines that allow the public to make informed decisions regarding its consumption.While marine fish have attractedmuch research interest due to their higher arsenic content,research on freshwater fish is limited due to the challenges in quantifying and identifying arsenic species present at trace levels.We describe here a sensitivemethod and its application to the quantification of arsenic species in freshwater fish.Arsenic species from fish tissues were extracted using a methanol/water mixture(1:1 vol.ratio)and ultrasound sonication.Anion-exchange high-performance liquid chromatography(HPLC)enabled separation of arsenobetaine(AsB),inorganic arsenite(iAs^(Ⅲ)),dimethylarsinic acid(DMA),monomethylarsonic acid(MMA),inorganic arsenate(iAs^(Ⅴ)),and three new arsenic species.Inductively coupled plasma mass spectrometry(ICPMS)provided highly sensitive and specific detection of arsenic.A limit of detection of 0.25μg/kg(wet weight fish tissue)was achieved for the five target arsenic species:AsB,iAs^(Ⅲ),DMA,MMA,and iAs^(Ⅴ).A series of experimentswere conducted to ensure the accuracy and validity of the analytical method.The method was successfully applied to the determination of arsenic species in lakewhitefish,northern pike,and walleye,with AsB,DMA,and iAs^(Ⅴ) being frequently detected.Three new arsenic species were detected,but their chromatographic retention times did not match with those of any available arsenic standards.Future research is necessary to elucidate the identity of these new arsenic species detected in freshwater fish.展开更多
As humanity enters the era of life sciences and artificial intelligence,an increasing number of biomedical challenges in are becoming associated with the biological activity of substances,the vast amounts of data and ...As humanity enters the era of life sciences and artificial intelligence,an increasing number of biomedical challenges in are becoming associated with the biological activity of substances,the vast amounts of data and the extent of understanding at the molecular level.Traditional methods that focus solely on the physical properties of substances are insufficient to address these challenges.Cell membrane chromatography(CMC)is a recognition and analysis method that simultaneously determines the biological activities and physical properties of substances under biomimetic conditions.The book of Cell Membrane Chromatography written by Prof.Langchong He et al.provides the evolution of chromatographic technology and an overview of intermolecular interactions,focusing on the CMC bionic testing system,CMC stationary phase,CMC analyzer,and typical applications.CMC serves as an effective tool for drug discovery and quality control in pharmaceutical field.展开更多
[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Method...[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Methods]An Inertsil ODS-C 18 column(250 mm×4.6 mm,5μm)was used.The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution(10:90).The flow rate was 1.0 mL/min.The detection wavelength was 274 nm.The column temperature was 25℃.The injection volume was 10μL.The content of three components,gallic acid,protocatechuic acid,and protocatechualdehyde,was determined in 13 batches of T.asiatica.[Results]Gallic acid showed good linearity within the range of 0.020-6.400μg/mL,protocatechuic acid within 0.201-6.432μg/mL,and protocatechualdehyde within 0.202-6.464μg/mL(r>0.9990).The average recovery rates ranged from 98.61%to 101.17%,with RSD s between 1.21%and 2.69%.[Conclusions]The quantitative determination method established in this study is simple and feasible,and can provide a basis for the quality evaluation of T.asiatica.展开更多
Quantitative structure-retention relationship(QSRR)is an important tool in chromatography.QSRR examines the correlation between molecular structures and their retention behaviors during chromatographic separation.This...Quantitative structure-retention relationship(QSRR)is an important tool in chromatography.QSRR examines the correlation between molecular structures and their retention behaviors during chromatographic separation.This approach involves developing models for predicting the retention time(RT)of analytes,thereby accelerating method development and facilitating compound identification.In addition,QSRR can be used to study compound retention mechanisms and support drug screening efforts.This review provides a comprehensive analysis of QSRR workflows and applications,with a special focus on the role of artificial intelligence-an area not thoroughly explored in previous reviews.Moreover,we discuss current limitations in RT prediction and propose promising solutions.Overall,this review offers a fresh perspective on future QSRR research,encouraging the development of innovative strategies that enable the diverse applications of QSRR models in chromatographic analysis.展开更多
[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromo...[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromogenic reactions of starch and dextrin,as well as the comparative study of thin-layer chromatography of oligosaccharides present in Jiulongteng honey.[Results]None of the 35 batches of Jiulongteng honey samples exhibited blue(indicating starch),green,or reddish-brown(indicating dextrin)coloration,suggesting that no adulterants such as artificially added starch,dextrin,or sugar were present in these samples.Furthermore,none of the 35 batches displayed additional spots below the corresponding positions of the control,indicating that the sugar composition was consistent with the oligosaccharide profile of natural honey.No components inconsistent with the oligosaccharide profile of natural honey were detected.Therefore,it can be concluded that the Jiulongteng honey samples in this experiment were pure and free from adulteration with starch,dextrin,or other sugar substances.[Conclusions]The method employed in this experiment is straightforward and quick to implement,effectively preventing adulterated honey from entering the market.It enhances the efficiency of quality control for Jiulongteng honey and promotes the healthy development of the Jiulongteng honey industry.展开更多
[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the e...[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the ethnomedicinal plant Eleutherine americana Merr.et K.Heyne.[Methods]The sample of E.americana bulbs was initially extracted with ethanol,followed by three successive extractions with ethyl acetate-water(2:1,V/V)to obtain the target component-enriched fraction.Eight solvent systems were systematically optimized,and a mixture of petroleum ether-ethyl acetate-ethanol-water(5:5:6:4,V/V/V/V)was identified as the optimal solvent system for high-speed counter-current chromatography(HSCCC)separation under conditions of 900 rpm,2 mL/min,and 35℃.The crude HSCCC product was further purified by silica gel column chromatography(200-300 mesh)using gradient elution with a solvent system of n-hexane-dichloromethane-ethyl acetate(varying from 10:5:1 to 4:5:1,V/V/V).UPLC-PDA(Agilent SB-C_(18)column)and nuclear magnetic resonance spectroscopy(600 MHz)were comprehensively employed to assess compound purity and confirm molecular structures.[Results]An optimized technique integrating HSCCC and silica gel column chromatography was established,successfully enabling the large-scale preparation of three bioactive components:eleutherol(purity 99%),eleutherine(purity 98%),and isoeleutherine(purity 98%).Structural identification results were consistent with those reported in the literature.Compared to traditional methods,the new approach demonstrated improved separation efficiency and reduced solvent consumption.[Conclusions]The combined separation method utilizing HSCCC and silica gel column chromatography established in this study demonstrates notable advantages,including high efficiency,environmental friendliness,and cost-effectiveness,enabling the large-scale preparation of the three major active components from E.americana.This approach outperforms conventional methods by offering higher separation efficiency,reduced solvent consumption,and superior product purity,providing a robust technical solution for the development and utilization of bioactive compounds from E.americana.Moreover,it offers a novel methodological reference for the isolation and purification of other natural products.展开更多
Mitochondria are fundamental organelles that play a crucial role in cellular energy metabolism,substance metabolism,and various essential cellular signaling pathways.The dysfunction of mitochondria is significantly im...Mitochondria are fundamental organelles that play a crucial role in cellular energy metabolism,substance metabolism,and various essential cellular signaling pathways.The dysfunction of mitochondria is significantly implicated in the onset and progression of aging,neurodegenerative diseases,metabolic disorders,and tumors,thereby rendering mitochondria-targeted regulation,a vital strategy for disease prevention and treatment.The recently developed mitochondrial membrane chromatography(MMC)technique,which immobilizes mitochondrial proteins as a chromatographic separation medium,has shown great potential for efficiently screening mitochondria-targeted modulators from complex compound library.In contrast to traditional screening methods,MMC has no need to purify mitochondrial proteins and can preserve its in situ and physiological conformation.Consequently,it presents broader application prospects for screening mitochondrial modulators as well as investigating receptor-ligand interactions involving any target protein associated with mitochondria.This review aims to elucidate the critical role of mitochondria in the development and progression of major chronic diseases,discuss recent advancements and applications of MMC,and propose future directions for MMC in the identification of novel mitochondrial modulators.展开更多
The rapid screening of bioactive constituents within traditional Chinese medicine(TCM)presents a significant challenge to researchers.Prevailing strategies for the screening of active components in TCM often overlook ...The rapid screening of bioactive constituents within traditional Chinese medicine(TCM)presents a significant challenge to researchers.Prevailing strategies for the screening of active components in TCM often overlook trace components owing to their concealment by more abundant constituents.To address this limitation,a fishing strategy based on offline two-dimensional liquid chromatography(2D-LC)combined with surface plasmon resonance(SPR)was utilized to screen bioactive trace components targeting peroxiredoxin 3(PRDX3),using Uncaria alkaloids(UAs)as a case study.Initially,an orthogonal preparative offline 2D-LC system combining a positively charged C_(18)column and a conventional C_(18)column under disparate mobile phase conditions was constructed.To fully reveal the trace alkaloids,132D fractions of UAs were prepared,and their components were characterized using mass spectrometry(MS).Subsequently,employing PRDX3 as the targeting protein,a SPR-based screening approach was established and rigorously validated with geissoschizine methyl ether(GSM)serving as a positive control for binding.Employing this refined strategy,29 candidate binding alkaloids were fished from the 132D fractions.Notably,combining offline 2D-LC with SPR increased the yield of candidate binding components from 10 to 29 when compared to SPR-based screening alone.Subsequent binding affinity assays confirmed that PRDX3 was a direct binding target for the 12 fished alkaloids,with isovallesiachotamine(IV),corynoxeine N-oxide(CO-N),and cadambine(CAD)demonstrating the highest affinity for PRDX3.Their interactions were further validated through molecular docking analysis.Subsequent intracellular H_(2)O_(2)measurement assays and transfection experiments confirmed that these three trace alkaloids enhanced PRDX3-mediated H_(2)O_(2)clearance.In conclusion,this study introduced an innovative strategy for the identification of active trace components in TCM.This approach holds promise for accelerating research on medicinal components within this field.展开更多
A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fr...A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.展开更多
Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,t...Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,the toxic components of P.multiflorum,during different processing cycles.We employed the ultra-high-performance liquid chromatography triple quadrupole mass spectrometry method to quantify six dianthrones in raw P.multiflorum and formulations processed with a method called nine cycles of steaming and sunning.Additionally,toxicity assessments were conducted using human normal liver cell line L02 and zebrafish embryos.Results:Results indicate a gradual reduction in dianthrones content with increasing processing cycles.Processed formulations exhibited significantly reduced cytotoxic-ity in L02 cells and hepatotoxicity in zebrafish embryos.Conclusions:Our findings elucidate the relationship between processing cycles and P.multiflorum toxicity,providing theoretical support for its safe use.展开更多
[Objective]The aim of this work was to establish an analytical method for the determination of deoxynivalenol(DON)in feeds using automatic immunomagnetic beads(IMBs)clean-up coupled with high-performance liquid chroma...[Objective]The aim of this work was to establish an analytical method for the determination of deoxynivalenol(DON)in feeds using automatic immunomagnetic beads(IMBs)clean-up coupled with high-performance liquid chromatography.[Method]Feed samples were extracted using ultra-pure water,purified by automatic IMBs,and subsequently analyzed via high-performance liquid chromatography,employing an external standard method for quantification.[Result]A satisfactory linearity was achieved for DON within the concentration range of 0.05 to 2.0μg/mL,with the corresponding correlation coefficients(R^(2))exceeding 0.9999.The limit of detection(LOD)and limit of quantification(LOQ)for the proposed method were determined to be 0.03 and 0.1 mg/kg,respectively.The average recoveries of the fortified samples(0.1,0.2 and 1.0 mg/kg)were 88.5%−100.6%,with the relative standard deviations(RSD)ranging from 2.1%to 9.7%.[Conclusion]In comparison with the traditional solidphase extraction and immunoaffinity column purification methods,the IMBs technique consolidates the extraction,separation,and purification into a single process.This approach enables fully automated processing,which significantly enhances work efficiency and mitigates result deviations that may arise from manual operations.Consequently,this technique is particularly well-suited for the determination of DON in a large number of feed samples.展开更多
Aim A novel method has been developed for evaluation of the levels of total residual protein in antibiotics produced by fermentation using gel filtration chromatography (GFC) combined with Bradford assay based on dete...Aim A novel method has been developed for evaluation of the levels of total residual protein in antibiotics produced by fermentation using gel filtration chromatography (GFC) combined with Bradford assay based on determination of residual protein in lincomycin hydrochloride. Methods The chromatographic conditions were SuperdexTM peptide column, 0.01 mol*L-1 phosphate buffer solution as mobile phase, and flow rate of 1 mL·min-1. Five hundred microliters of lincomycin hydrochloride solution (3 g of lincomycin hydrochloride dissolved in 10 mL of mobile phase) was injected into the chromatograph and the eluted solution was collected between 6 min and 14.5 min (protein eluted from column within this period), and the residual content of total protein in the eluted solution was assayed using Bradford assay method. Results The average recovery was more than 90% for bovine serum albumin, the calibration equation for the range of 0-12 μg·mL-1 of protein was y=-0.002 4x2+0.064 2x+0.002 9, r2=0.999 9, RSD=0.1%-0.9%, and the LOD and LOQ were 3 and 10 ng·mL-1 of protein, respectively. Conclusion The novel method for determining the residual protein in ferment antibio-tics is simple, rapid, and precise.展开更多
Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic...Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic acid, homovanillic acid and 5-hydroxyindole-3-acetic acid） in different brain subregions of rats using a newly developed simple, sensitive and selective high-performance liquid chromatography with fluorescence detection （HPLC-FLD） method. In this new HPLC-FLD method, analytes were directly extracted and separated without deriveatization step within 20 min. The FLD wavelength was set at 280 nm and 330 nm for excitation and emission, respectively. The analytes were separated on an Agilent Eclipse Plus Cls column （4.6 mm×150 mm, 5.0 μm） equipped with an Agilent XDB-C18 security guard column （4.6 mm×12.5 mm, 5.0 lam）, and the column temperature was maintained at 35 ℃. The mobile phase for elution was isocratic. The mobile phase consisted of citric acid buffer （50 mmol/L citric acid, 50 mmol/L sodium acetate, 0.5 mmol/L octane sulfonic acid sodium salt, 0.5 mmol/L Na2EDTA and 5 mmol/L triethylamine, pH 3.8） and methanol （90：10, v/v） at a flow rate of 1.0 mL/min. The detection limit （DL） was 0.9-23 nM for all the MANTs and their metabolites with a sample volume of 50 μL. The method was shown to be highly reproducible in terms of peak area （intraday, 0.08%-1.85% RSD, n = 5）. The simultaneous measurement of these MANTs and their metabolites improved our understanding of the neurochemistry in the central nervous system （CNS） in relation to different addictive drugs （methamphetamine, heroin and their mixture） in drug-addicted rat models.展开更多
基金supported by the National Natural Science Foundation of China (Nos.22064020,22364022,and 22174125)the Applied Basic Research Foundation of Yunnan Province (Nos.202101AT070101 and 202201AT070029)。
文摘Developing a chiral material as versatile and universal chiral stationary phase(CSP) for chiral separation in diverse chromatographic techniques simultaneously is of great significance.In this study,we demonstrated for the first time that a chiral metal-organic cage(MOC),[Zn_(6)M_(4)],as a universal chiral recognition material for both multi-mode high-performance liquid chromatography(HPLC) and capillary gas chromatography(GC) enantioseparation.Two novel HPLC CSPs with different bonding arms(CSP-A with a cationic imidazolium bonding arm and CSP-B with an alkyl chain bonding arm) were prepared by clicking of functionalized chiral MOC [Zn_(6)M_(4)] onto thiolated silica via thiol-ene click chemistry.Meanwhile,a capillary GC column statically coated with the chiral MOC [Zn_(6)M_(4)] was also fabricated.The results showed that the chiral MOC exhibits excellent enantioselectivity not only in normal phase HPLC(NP-HPLC) and reversed phase(RP-HPLC) but also in GC,and various racemates were well separated,including alcohols,diols,esters,ketones,ethers,amines,and epoxides.Importantly,CSP-A and CSP-B are complementary to commercially available Chiralcel OD-H and Chiralpak AD-H columns in enantioseparation,which can separate some racemates that could not be or could not well be separated by the two widely used commercial columns,suggesting the great potential of the two prepared CSPs in enantioseparation.This work reveals that the chiral MOC is potential versatile chiral recognition materials for both HPLC and GC,and also paves the way to expand the potential applications of MOCs.
基金supported by National Natural Science Foundation of China (Nos.21906124,32302202)Natural Science Foundation of Hubei Province (No.2017CFB220)Natural Science Foundation of Shandong Province (No.ZR2023MH278)。
文摘Metal organic framework(MOF) assembled with coordination bonds has the disadvantage of poor stability that limits its application in the field of stationary phase,while covalent organic framework(COF)assembled through covalent bonds exhibits excellent structural stability.It has been shown that the stationary phases prepared by combining MOF and COF can make up for the poor stability of MOF@SiO_(2),and the MOF/COF composites have superior chromatographic separation performance.However,the traditional methods for preparing COF/MOF based stationary phases are generally solvent thermal synthesis.In this study,a green and low-cost synthesis method was proposed for the preparation of MOF/COF@SiO_(2) stationary phase.Firstly,COF@SiO_(2) was prepared in a choline chloride/ethylene glycol based deep eutectic solvent(DES).Secondly,another acid-base tunable DES prepared by mixing p-toluenesulfonic acid(PTSA)and 2-methylimidazole in different proportions was introduced as the reaction solvent and reactant for rapid synthesis of MOF/COF@SiO_(2).Compared with the toxic transition metal-based MOFs selected in most previous studies,a lightweight and non-toxic S-zone metal(calcium) based MOF was employed in this study.PTSA and calcium will form the calcium/oxygen-containing organic acid framework in acidic DES,which assembles with terephthalic acid dissolved in basic DES to form MOF.The strong hydrogen bonding effect of DES can facilitate rapid assembly of Ca-MOF.The obtained Ca-MOF/COF@SiO_(2) can be used for multi-mode chromatography to efficiently separate multiple isomeric/hydrophilic/hydrophobic analytes.The synthesis method of Ca-MOF/COF@SiO_(2) is green and mild,especially the use of acid-base tunable DES promotes the rapid synthesis of non-toxic Ca-MOF/COF@silica composites,which offers an innovative approach of greenly synthesizing novel MOF/COF stationary phases and extends their applications in the field of chromatography.
基金supported by Alberta Health,Alberta Innovates,the Canada Research Chairs Program,the Canadian Institutes of Health Research,and the Natural Sciences and Engineering Research Council of Canada。
文摘Arsenic speciation in freshwater fish is crucial for providing meaningful consumption guidelines that allow the public to make informed decisions regarding its consumption.While marine fish have attractedmuch research interest due to their higher arsenic content,research on freshwater fish is limited due to the challenges in quantifying and identifying arsenic species present at trace levels.We describe here a sensitivemethod and its application to the quantification of arsenic species in freshwater fish.Arsenic species from fish tissues were extracted using a methanol/water mixture(1:1 vol.ratio)and ultrasound sonication.Anion-exchange high-performance liquid chromatography(HPLC)enabled separation of arsenobetaine(AsB),inorganic arsenite(iAs^(Ⅲ)),dimethylarsinic acid(DMA),monomethylarsonic acid(MMA),inorganic arsenate(iAs^(Ⅴ)),and three new arsenic species.Inductively coupled plasma mass spectrometry(ICPMS)provided highly sensitive and specific detection of arsenic.A limit of detection of 0.25μg/kg(wet weight fish tissue)was achieved for the five target arsenic species:AsB,iAs^(Ⅲ),DMA,MMA,and iAs^(Ⅴ).A series of experimentswere conducted to ensure the accuracy and validity of the analytical method.The method was successfully applied to the determination of arsenic species in lakewhitefish,northern pike,and walleye,with AsB,DMA,and iAs^(Ⅴ) being frequently detected.Three new arsenic species were detected,but their chromatographic retention times did not match with those of any available arsenic standards.Future research is necessary to elucidate the identity of these new arsenic species detected in freshwater fish.
文摘As humanity enters the era of life sciences and artificial intelligence,an increasing number of biomedical challenges in are becoming associated with the biological activity of substances,the vast amounts of data and the extent of understanding at the molecular level.Traditional methods that focus solely on the physical properties of substances are insufficient to address these challenges.Cell membrane chromatography(CMC)is a recognition and analysis method that simultaneously determines the biological activities and physical properties of substances under biomimetic conditions.The book of Cell Membrane Chromatography written by Prof.Langchong He et al.provides the evolution of chromatographic technology and an overview of intermolecular interactions,focusing on the CMC bionic testing system,CMC stationary phase,CMC analyzer,and typical applications.CMC serves as an effective tool for drug discovery and quality control in pharmaceutical field.
基金Supported by Regional Science Foundation of China,National Natural Science Foundation(No.82160820)General Program of Guizhou Provincial Natural Science Foundation[QianKeHe Foundation-ZK(2023)General153].
文摘[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Methods]An Inertsil ODS-C 18 column(250 mm×4.6 mm,5μm)was used.The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution(10:90).The flow rate was 1.0 mL/min.The detection wavelength was 274 nm.The column temperature was 25℃.The injection volume was 10μL.The content of three components,gallic acid,protocatechuic acid,and protocatechualdehyde,was determined in 13 batches of T.asiatica.[Results]Gallic acid showed good linearity within the range of 0.020-6.400μg/mL,protocatechuic acid within 0.201-6.432μg/mL,and protocatechualdehyde within 0.202-6.464μg/mL(r>0.9990).The average recovery rates ranged from 98.61%to 101.17%,with RSD s between 1.21%and 2.69%.[Conclusions]The quantitative determination method established in this study is simple and feasible,and can provide a basis for the quality evaluation of T.asiatica.
基金supported by the Shanghai Sailing Program,China(Grant No.:23YF1413300).
文摘Quantitative structure-retention relationship(QSRR)is an important tool in chromatography.QSRR examines the correlation between molecular structures and their retention behaviors during chromatographic separation.This approach involves developing models for predicting the retention time(RT)of analytes,thereby accelerating method development and facilitating compound identification.In addition,QSRR can be used to study compound retention mechanisms and support drug screening efforts.This review provides a comprehensive analysis of QSRR workflows and applications,with a special focus on the role of artificial intelligence-an area not thoroughly explored in previous reviews.Moreover,we discuss current limitations in RT prediction and propose promising solutions.Overall,this review offers a fresh perspective on future QSRR research,encouraging the development of innovative strategies that enable the diverse applications of QSRR models in chromatographic analysis.
基金Supported by Enhancement Project of Basic Scientific Research Ability of Young and Middle-aged Teachers in Guangxi Universities(2020KY07040)School-level Scientific Research Project of Guangxi University of Chinese Medicine(2024QN022)Self-financed Scientific Research Project of Guangxi Zhuang Autonomous Region Administration of Traditional Chinese Medicine(GXZYL20240818).
文摘[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromogenic reactions of starch and dextrin,as well as the comparative study of thin-layer chromatography of oligosaccharides present in Jiulongteng honey.[Results]None of the 35 batches of Jiulongteng honey samples exhibited blue(indicating starch),green,or reddish-brown(indicating dextrin)coloration,suggesting that no adulterants such as artificially added starch,dextrin,or sugar were present in these samples.Furthermore,none of the 35 batches displayed additional spots below the corresponding positions of the control,indicating that the sugar composition was consistent with the oligosaccharide profile of natural honey.No components inconsistent with the oligosaccharide profile of natural honey were detected.Therefore,it can be concluded that the Jiulongteng honey samples in this experiment were pure and free from adulteration with starch,dextrin,or other sugar substances.[Conclusions]The method employed in this experiment is straightforward and quick to implement,effectively preventing adulterated honey from entering the market.It enhances the efficiency of quality control for Jiulongteng honey and promotes the healthy development of the Jiulongteng honey industry.
基金Supported by Natural Science Foundation of Tibet Autonomous Region,Science and Technology Department of Tibet(XZ202501ZR0118).
文摘[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the ethnomedicinal plant Eleutherine americana Merr.et K.Heyne.[Methods]The sample of E.americana bulbs was initially extracted with ethanol,followed by three successive extractions with ethyl acetate-water(2:1,V/V)to obtain the target component-enriched fraction.Eight solvent systems were systematically optimized,and a mixture of petroleum ether-ethyl acetate-ethanol-water(5:5:6:4,V/V/V/V)was identified as the optimal solvent system for high-speed counter-current chromatography(HSCCC)separation under conditions of 900 rpm,2 mL/min,and 35℃.The crude HSCCC product was further purified by silica gel column chromatography(200-300 mesh)using gradient elution with a solvent system of n-hexane-dichloromethane-ethyl acetate(varying from 10:5:1 to 4:5:1,V/V/V).UPLC-PDA(Agilent SB-C_(18)column)and nuclear magnetic resonance spectroscopy(600 MHz)were comprehensively employed to assess compound purity and confirm molecular structures.[Results]An optimized technique integrating HSCCC and silica gel column chromatography was established,successfully enabling the large-scale preparation of three bioactive components:eleutherol(purity 99%),eleutherine(purity 98%),and isoeleutherine(purity 98%).Structural identification results were consistent with those reported in the literature.Compared to traditional methods,the new approach demonstrated improved separation efficiency and reduced solvent consumption.[Conclusions]The combined separation method utilizing HSCCC and silica gel column chromatography established in this study demonstrates notable advantages,including high efficiency,environmental friendliness,and cost-effectiveness,enabling the large-scale preparation of the three major active components from E.americana.This approach outperforms conventional methods by offering higher separation efficiency,reduced solvent consumption,and superior product purity,providing a robust technical solution for the development and utilization of bioactive compounds from E.americana.Moreover,it offers a novel methodological reference for the isolation and purification of other natural products.
基金financially supported by,the Space Medical Experiment Project of China Manned Space Program(Program No.:HYZHXM01023)the National Natural Science Foundation of China(Grant No.:31870848)+1 种基金the National foreign experts project(Grant No.:G2022170026L)Key R&D Program of Shaanxi Province(Grant Nos.:2021GXLH-Z-064&2024SF-ZDCYL-03-24).
文摘Mitochondria are fundamental organelles that play a crucial role in cellular energy metabolism,substance metabolism,and various essential cellular signaling pathways.The dysfunction of mitochondria is significantly implicated in the onset and progression of aging,neurodegenerative diseases,metabolic disorders,and tumors,thereby rendering mitochondria-targeted regulation,a vital strategy for disease prevention and treatment.The recently developed mitochondrial membrane chromatography(MMC)technique,which immobilizes mitochondrial proteins as a chromatographic separation medium,has shown great potential for efficiently screening mitochondria-targeted modulators from complex compound library.In contrast to traditional screening methods,MMC has no need to purify mitochondrial proteins and can preserve its in situ and physiological conformation.Consequently,it presents broader application prospects for screening mitochondrial modulators as well as investigating receptor-ligand interactions involving any target protein associated with mitochondria.This review aims to elucidate the critical role of mitochondria in the development and progression of major chronic diseases,discuss recent advancements and applications of MMC,and propose future directions for MMC in the identification of novel mitochondrial modulators.
基金supported by Shanghai Institute of Materia Medica-Shanghai University of Traditional Chinese Medicine(SIMM-SHUTCM)Traditional Chinese Medicine Innovation Joint Research Program,China(Grant No.:2022,E2G808H096)the National Key Research and Development Program of China(Grant Nos.:2022YFC3501704 and 2023YFC3504205)Sanming Project of Medicine in Shenzhen,China(Grant No.:ZZYSM202106004).
文摘The rapid screening of bioactive constituents within traditional Chinese medicine(TCM)presents a significant challenge to researchers.Prevailing strategies for the screening of active components in TCM often overlook trace components owing to their concealment by more abundant constituents.To address this limitation,a fishing strategy based on offline two-dimensional liquid chromatography(2D-LC)combined with surface plasmon resonance(SPR)was utilized to screen bioactive trace components targeting peroxiredoxin 3(PRDX3),using Uncaria alkaloids(UAs)as a case study.Initially,an orthogonal preparative offline 2D-LC system combining a positively charged C_(18)column and a conventional C_(18)column under disparate mobile phase conditions was constructed.To fully reveal the trace alkaloids,132D fractions of UAs were prepared,and their components were characterized using mass spectrometry(MS).Subsequently,employing PRDX3 as the targeting protein,a SPR-based screening approach was established and rigorously validated with geissoschizine methyl ether(GSM)serving as a positive control for binding.Employing this refined strategy,29 candidate binding alkaloids were fished from the 132D fractions.Notably,combining offline 2D-LC with SPR increased the yield of candidate binding components from 10 to 29 when compared to SPR-based screening alone.Subsequent binding affinity assays confirmed that PRDX3 was a direct binding target for the 12 fished alkaloids,with isovallesiachotamine(IV),corynoxeine N-oxide(CO-N),and cadambine(CAD)demonstrating the highest affinity for PRDX3.Their interactions were further validated through molecular docking analysis.Subsequent intracellular H_(2)O_(2)measurement assays and transfection experiments confirmed that these three trace alkaloids enhanced PRDX3-mediated H_(2)O_(2)clearance.In conclusion,this study introduced an innovative strategy for the identification of active trace components in TCM.This approach holds promise for accelerating research on medicinal components within this field.
文摘A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.
基金National Natural Science Foundation of China,Grant/Award Number:81973476Chinese Society of Toxicology,Grant/Award Number:CST2021CT101。
文摘Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,the toxic components of P.multiflorum,during different processing cycles.We employed the ultra-high-performance liquid chromatography triple quadrupole mass spectrometry method to quantify six dianthrones in raw P.multiflorum and formulations processed with a method called nine cycles of steaming and sunning.Additionally,toxicity assessments were conducted using human normal liver cell line L02 and zebrafish embryos.Results:Results indicate a gradual reduction in dianthrones content with increasing processing cycles.Processed formulations exhibited significantly reduced cytotoxic-ity in L02 cells and hepatotoxicity in zebrafish embryos.Conclusions:Our findings elucidate the relationship between processing cycles and P.multiflorum toxicity,providing theoretical support for its safe use.
基金Supported by National Key Research and Development Program of China(2023YFD1301001)Central Public-interest Scientific Institution Basal Research Fund(1610072023005)Agricultural Science and Technology Innovation Program of CAAS(CAAS-ASTIP-IQSTAP-04).
文摘[Objective]The aim of this work was to establish an analytical method for the determination of deoxynivalenol(DON)in feeds using automatic immunomagnetic beads(IMBs)clean-up coupled with high-performance liquid chromatography.[Method]Feed samples were extracted using ultra-pure water,purified by automatic IMBs,and subsequently analyzed via high-performance liquid chromatography,employing an external standard method for quantification.[Result]A satisfactory linearity was achieved for DON within the concentration range of 0.05 to 2.0μg/mL,with the corresponding correlation coefficients(R^(2))exceeding 0.9999.The limit of detection(LOD)and limit of quantification(LOQ)for the proposed method were determined to be 0.03 and 0.1 mg/kg,respectively.The average recoveries of the fortified samples(0.1,0.2 and 1.0 mg/kg)were 88.5%−100.6%,with the relative standard deviations(RSD)ranging from 2.1%to 9.7%.[Conclusion]In comparison with the traditional solidphase extraction and immunoaffinity column purification methods,the IMBs technique consolidates the extraction,separation,and purification into a single process.This approach enables fully automated processing,which significantly enhances work efficiency and mitigates result deviations that may arise from manual operations.Consequently,this technique is particularly well-suited for the determination of DON in a large number of feed samples.
文摘Aim A novel method has been developed for evaluation of the levels of total residual protein in antibiotics produced by fermentation using gel filtration chromatography (GFC) combined with Bradford assay based on determination of residual protein in lincomycin hydrochloride. Methods The chromatographic conditions were SuperdexTM peptide column, 0.01 mol*L-1 phosphate buffer solution as mobile phase, and flow rate of 1 mL·min-1. Five hundred microliters of lincomycin hydrochloride solution (3 g of lincomycin hydrochloride dissolved in 10 mL of mobile phase) was injected into the chromatograph and the eluted solution was collected between 6 min and 14.5 min (protein eluted from column within this period), and the residual content of total protein in the eluted solution was assayed using Bradford assay method. Results The average recovery was more than 90% for bovine serum albumin, the calibration equation for the range of 0-12 μg·mL-1 of protein was y=-0.002 4x2+0.064 2x+0.002 9, r2=0.999 9, RSD=0.1%-0.9%, and the LOD and LOQ were 3 and 10 ng·mL-1 of protein, respectively. Conclusion The novel method for determining the residual protein in ferment antibio-tics is simple, rapid, and precise.
基金National Natural Science Foundation(Grant No.813 73372)the Open Foundation of State Key Laboratory of Natural and Biomimetic Drugs(Grant No.SKL2012004)Specialized Research Fund for the Doctoral Program of Higher Education of China(Grant No.20110001110021 and 20130001110059)
文摘Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic acid, homovanillic acid and 5-hydroxyindole-3-acetic acid） in different brain subregions of rats using a newly developed simple, sensitive and selective high-performance liquid chromatography with fluorescence detection （HPLC-FLD） method. In this new HPLC-FLD method, analytes were directly extracted and separated without deriveatization step within 20 min. The FLD wavelength was set at 280 nm and 330 nm for excitation and emission, respectively. The analytes were separated on an Agilent Eclipse Plus Cls column （4.6 mm×150 mm, 5.0 μm） equipped with an Agilent XDB-C18 security guard column （4.6 mm×12.5 mm, 5.0 lam）, and the column temperature was maintained at 35 ℃. The mobile phase for elution was isocratic. The mobile phase consisted of citric acid buffer （50 mmol/L citric acid, 50 mmol/L sodium acetate, 0.5 mmol/L octane sulfonic acid sodium salt, 0.5 mmol/L Na2EDTA and 5 mmol/L triethylamine, pH 3.8） and methanol （90：10, v/v） at a flow rate of 1.0 mL/min. The detection limit （DL） was 0.9-23 nM for all the MANTs and their metabolites with a sample volume of 50 μL. The method was shown to be highly reproducible in terms of peak area （intraday, 0.08%-1.85% RSD, n = 5）. The simultaneous measurement of these MANTs and their metabolites improved our understanding of the neurochemistry in the central nervous system （CNS） in relation to different addictive drugs （methamphetamine, heroin and their mixture） in drug-addicted rat models.
