[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
Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morpho...Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morphology,good monodispersity and high specific surface area,were used as a stationary phase for high-performance liquid chromatography(HPLC).The single-crystal 3D COFs packed column not only exhibits high efficiency in separating hydrophobic molecules involving substituted benzenes,halogenated benzenes,halogenated nitrobenzenes,aromatic amines,aromatic hydrocarbons(PAHs)and phthalate esters(PAEs),but also achieves baseline separation of acenaphthene and acenaphthylene with similar physical and chemical properties as well as environmental pollutants,which cannot be quickly separated on commercial C18 column and a polycrystalline 3D COFs packed column.Especially,the column efficiency of 17303-24255 plates/m was obtained for PAEs,and the resolution values for acenaphthene and acenaphthylene,and carbamazepine(CBZ)and carbamazepine-10,11-epoxide(CBZEP)were 1.7and 2.2,respectively.This successful application not only confirmed the great potential of the singlecrystal 3D COFs in HPLC separation of the organic molecules,but also facilitates the application of COFs in separation science.展开更多
High-entropy alloy(HEA)offer tunable composition and surface structures,enabling the creation of novel active sites that enhance catalytic performance in renewable energy application.However,the inherent surface compl...High-entropy alloy(HEA)offer tunable composition and surface structures,enabling the creation of novel active sites that enhance catalytic performance in renewable energy application.However,the inherent surface complexity and tendency for elemental segregation,which results in discrepancies between bulk and surface compositions,pose challenges for direct investigation via density functional theory.To address this,Monte Carlo simulations combined with molecular dynamics were employed to model surface segregation across a broad range of elements,including Cu,Ag,Au,Pt,Pd,and Al.The analysis revealed a trend in surface segregation propensity following the order Ag>Au>Al>Cu>Pd>Pt.To capture the correlation between surface site characteristics and the free energy of multi-dentate CO_(2)reduction intermediates,a graph neural network was designed,where adsorbates were transformed into pseudo-atoms at their centers of mass.This model achieved mean absolute errors of 0.08–0.15 eV for the free energies of C_(2)intermediates,enabling precise site activity quantification.Results indicated that increasing the concentration of Cu,Ag,and Al significantly boosts activity for CO and C_(2)formation,whereas Au,Pd,and Pt exhibit negative effects.By screening stable composition space,promising HEA bulk compositions for CO,HCOOH,and C_(2)products were predicted,offering superior catalytic activity compared to pure Cu catalysts.展开更多
A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed a...A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.展开更多
In order to investigate the effects of two mineral admixtures （i. e., fly ash and ground slag）on initial defects existing in concrete microstructures, a high-resolution X-ray micro-CT（ micro-focus computer tomogra...In order to investigate the effects of two mineral admixtures （i. e., fly ash and ground slag）on initial defects existing in concrete microstructures, a high-resolution X-ray micro-CT（ micro-focus computer tomography）is employed to quantitatively analyze the initial defects in four series of highperformance concrete （HPC）specimens with additions of different mineral admixtures. The nigh-resolution 3D images of microstructures and filtered defects are reconstructed by micro- CT software. The size distribution and volume fractions of initial defects are analyzed based on 3D and 2D micro-CT images. The analysis results are verified by experimental results of watersuction tests. The results show that the additions of mineral admixtures in concrete as cementitious materials greatly change the geometrical properties of the microstructures and the spatial features of defects by physical-chemistry actions of these mineral admixtures. This is the major cause of the differences between the mechanical behaviors of HPC with and without mineral admixtures when the water-to-binder ratio and the size distribution of aggregates are constant.展开更多
The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and pr...The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs, a simple, easy, and sensitive high-performance liquid chromatography coupled with diode array detectors was developed for simultaneous determination of nine bioactive components in the herbal pairs. The calibration curve exhibited good linearity（r2≥0.9992）. The LODs and LOQs were ≤7.30 and 11.53 μg/m L, respectively. The intra-, inter-day and repeatability RSD values of the nine compounds were less than 3.86%, 2.71%, and 4.29%, respectively. The RSD stability values were less than 3.64%. The recovery of the method was in the range of 96.70%–102.10%, with RSD values less than 3.52%. The developed method can be applied to the intrinsic quality control of crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs.展开更多
The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture...The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture of chloroform-n-heptane.2-(4-Hydrazinocarbonyl- phenyl)-4,5-diphenylimidazole (HCPI) was used as a fluorescent labelling reagent of the fatty acids. The labelling reaction was carried out at 30℃ for 1 h at pH 6.5 and the resulting reaction mixture was sudjected to HPLC. The labelled fatty acid C_(17)(P-C_(17))was used as the internal standard. The la- belled fatty acids C_(16) and C_(18) were separated within 18 min on an ODS-8OTM column (150 mm× 6 mm ID,5μm,Tosoh Japan).The calibrlation curves of fatty acids from the spiked control serum were Y_1=-0.003 7 + 0.0028X_1,r=0.994 for FA C_( 16) and Y_2=0.00 1 2 + 0.00098X_2,r=0.999 for FA C_( 18),respectively.The average recoveries of facids from the spiked contrl serum were 107.2%(n=8,RSD=4.3%)for FA C_(16) and 97.35%(n=8, RSD=4.0%)for FA C_(18),respectively.The lower detection limits of fatty acids after reaction were 12μmol per 20μl injection for FA C_(16) and 18 μmol per 20μl injection for FA C_(18),respectively(signal to noise ratio, S/N=2).The HPLC/CL method was applied to the determination of FA C_(16) and FA C_(18) in normal human serum and the results showed that the concentrations of fatty acids in normal human serum were 0.134 ± 0.009 μ mol/ml serum(n=5) for FA C_(16) and 0.052±0.028 μmol/ml serum(n=5)for FA C_(18),respectively.展开更多
We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column usin...We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid （TFA） aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL （r2= 0.9998）, 9.38-1407 μg/mL （rz = 0.9999）, 80.6-8060μg/mL （r2 = 0.9999） and 2.10---630μg/mL （r2 = 0.9987） with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.展开更多
Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-A...Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-Aq column using a gradient elution with mobile phase of 8 mmol^L-1 ammonium acetate aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL·min^-1 at 25 ℃ with the diode-array detection at 260 nm. Results Cytidine, uridine, guanosine, adenosine and uracil had good linearity in the ranges of 1.79 - 57.40 μg·mL^-1 （r^2 = 1.0000）, 3.30 - 105.60 μg·mL^-1 （r^2 = 1.0000）, 3.09 - 98.80 μg·mL^ -1（r^2 = 0.9999）, 2.77 - 88.60 μg·mL^-1 （r^2 = 1.0000） and 0.38 - 12.30 μg·mL ^-1 （r^2 = 1.0000） with average recoveries of 93.9%, 96.5%, 92.7%, 93.2% and 98.8%, respectively. The content of cytidine, uridine, guanosine, adenosine and uracil in different parts of P. notogingeng were significantly different. Conclusion This is the first report on quantitative determination of nucleosides and nucleobases in P notoginseng.展开更多
The compositions and contents of ginsenbsides in Panax ginseng,P.quinquefolium and P.notoginseng were determined and compared by reversed-phase High-Performance Liquid Chro- matography(HPLC).The method was performed o...The compositions and contents of ginsenbsides in Panax ginseng,P.quinquefolium and P.notoginseng were determined and compared by reversed-phase High-Performance Liquid Chro- matography(HPLC).The method was performed on an Alltech Adsorbosphere HS C_(18) column,using 5×10^(-3)M NaH_2PO_4-H_3PO_4 buffer solution(pH 3.0)and acetonitrile-water(50:50)as gradient eluents. The baseline separation of ginsenosides Rb_1,Rb_2,Rb_1,Rc,Rd,Rf,Ro,and Re+Rg_1 was obtained in one analytical run.The ginsenosides are directly detected at 203 nm.The detection limit is 40μg at a signal to noise ratio of 3:1.The improved sample preparation and clean-up prior to injection with SEP-PAK C_(18)cartridge strongly reduced the front peaks caused by the impurities in the methanolic extracts of samples to afford a smooth baseline and clear background.The HPLC patterns of methanolic extracts mainly including the ginsenosides were found capable of serving as chemical fingerprints to differentiate the three species from each other.It was also found that there are no significant diffe- rences of the HPLC patterns between the wild Panax ginseng and the cultivated,the white and the red ginsengs,Chinese and Korean red ginsengs,and the tap roots of Panax ginseng collected in four consecutive months,only certain differences in contents of ginsenosides do exist.The contents of the nine major ginsenosides present in the rhizome,tap root and rootlet as well as the leaf of Panax quinquefolium were also determined and compared.展开更多
AIM: To perform plasma free amino acid (PFAA) profiling of esophageal squamous cell carcinoma (ESCC) patients at different pathological stages and healthy subjects.
The various advantages of organic polymer monoliths, including relatively simple preparation processes,abundant monomer availability, and a wide application range of pH, have attracted the attention of chromatographer...The various advantages of organic polymer monoliths, including relatively simple preparation processes,abundant monomer availability, and a wide application range of pH, have attracted the attention of chromatographers. Organic polymer monoliths prepared by traditional methods only have macropores and mesopores, and micropores of less than 50 nm are not commonly available. These typical monoliths are suitable for the separation of biological macromolecules such as proteins and nucleic acids, but their ability to separate small molecular compounds is poor. In recent years, researchers have successfully modified polymer monoliths to achieve uniform compact pore structures. In particular, microporous materials with pores of 50 nm or less that can provide a large enough surface area are the key to the separation of small molecules. In this review, preparation methods of polymer monoliths for high-performance liquid chromatography, including ultra-high cross-linking technology, post-surface modification, and the addition of nanomaterials, are discussed. Modified monolithic columns have been used successfully to separate small molecules with obvious improvements in column efficiency.展开更多
A high-performance liquid chromatography （HPLC） system was used in the reversed phase mode for the determination ofbenzalkonium chloride （BKC） in azithromycin viscous ophthalmic drops. A Venusil-XBP（L）-C18 （150...A high-performance liquid chromatography （HPLC） system was used in the reversed phase mode for the determination ofbenzalkonium chloride （BKC） in azithromycin viscous ophthalmic drops. A Venusil-XBP（L）-C18 （150 mm×4.6 mm, 5 gm） column was used at 50℃. The mobile phase consisted of a mixture of methanol-potassium phosphate （16：5, v/v）. Two sample preparation methods were compared. The results suggested that, compared with an extraction procedure, a deproteinization procedure was much quicker and more convenient. Using the deproteinization procedure for sample preparation, calibration curves were linear in the range 5.0-50μg/ml. The within-day and inter-day coefficients of variation were less than 10%. The average recoveries were determined as 96.70%, 98.52%, and 97.96% at concentrations of 10.0, 30.0, and 50.0 μg/ml, respectively. Variability in precision did not exceed 5%. In conclusion, this HPLC method using a simple sample treatment procedure appears suitable for monitoring BKC content in azithromycin viscous ophthalmic drops.展开更多
Camellia seed oil （CSO） is rich in oleic acid and has a high number of active components, which give the oil high nutritional value and a variety of biological activity. The aim of the present study was to determine...Camellia seed oil （CSO） is rich in oleic acid and has a high number of active components, which give the oil high nutritional value and a variety of biological activity. The aim of the present study was to determine the changes in the content and distribution of total polar compounds （TPC） in CSO during heating. TPC were isolated by means of preparative flash chromatography and further analyzed by high-performance size-exclusion chromatography （HPSEC） The TPC content of CSO increased from 4.74% to 25.29%, showing a significantly lower formation rate as compared to that of extra virgin olive oil （EVOO） and soybean oil （SBO） during heating. Furthermore, heating also resulted in significant differences （P〈0.05） in the distribution of TPC among these oils. Though the content of oxidized triacyl- glycerol dimers, oxidized triacylglycerol oligomers, and oxidized triacylglycerol monomers significantly increased in all these oils, their increased percentages were much less in CSO than those in EVOO, indicating that CSO has a greater ability to resist oxidation. This work may be useful for the food oil industry and consumers in helping to choose the correct oil and to decide on the useful lifetime of the oil.展开更多
Creatinine, uric acid, hypoxanthine and xanthine are important diagnostic biomarkers in human urine for gouty arthritis or renal disease diacrisis. A simple method for simultaneous determination of these biomarkers in...Creatinine, uric acid, hypoxanthine and xanthine are important diagnostic biomarkers in human urine for gouty arthritis or renal disease diacrisis. A simple method for simultaneous determination of these biomarkers in urine based on reversed-phase high-performance liquid chromatography （RP-HPLC） with ultraviolet （UV） detector was proposed. After pretreatment by dilution, centrifugation and filtration, the biomarkers in urine samples were separated by ODS-BP column by elution with methanol/50 mM NaH2PO4 buffer solution at pH 5.26 （5：95）. Good linearity between peak areas and concentrations of standards was obtained for the biomarkers with correlation coefficients in the range of 0.9957-0.9993. The proposed analytical method has satisfactory repeatability （the recovery of data in a range of creatinine, uric acid, hypoxanthine and xanthine was 93.49-97.90%, 95.38-96.45%, 112.46-115.78%and 90.82-97.13%with standard deviation of o5%, respectively） and the limits of detection （LODs, S/N Z 3） for creatinine, uric acid, hypoxanthine, and xanthine were 0.010, 0.025, 0.050 and 0.025 mg/L, respectively. The established method was proved to be simple, accurate, sensitive and reliable for the quantitation of gouty arthritis＇ biomarkers in human urine samples. The ratio of creatinine to uric acid was found to be a possible factor for assessment of gouty arthritis.展开更多
Aim A reliable high-performance liquid chromatographic (HPLC) method wasdeveloped for determination of germacrone in rat plasma. Methods The plasma samples were treatedwith acetonitrile and analyzed by HPLC with UV de...Aim A reliable high-performance liquid chromatographic (HPLC) method wasdeveloped for determination of germacrone in rat plasma. Methods The plasma samples were treatedwith acetonitrile and analyzed by HPLC with UV detection at 244 nm. Results The limit of detectionwas 100 ng·mL^(-1) for germacrone in plasma and the linear range was 0.1004-15.06 μg·mL^(-1) inplasma. The RSD of intra-day and inter-day assay was 1.87% - 4.29% and 1.29% -5.15%, respectively.The recoveries of germacrone were over 95%. The endogenous substances in plasma did not show anyinterference in the analysis. Conclusion The method is accurate and convenient, and suitable forpharmacokinetic studies of germacrone in rats.展开更多
A simple method has been proposed for the determination of clozapine （CLZ） and chlorpromazine （CPZ） in human urine by dispersive liquid-liquid microextraction （DLLME） in combination with high-performance liquid ...A simple method has been proposed for the determination of clozapine （CLZ） and chlorpromazine （CPZ） in human urine by dispersive liquid-liquid microextraction （DLLME） in combination with high-performance liquid chromatography-ultraviolet detector （HPLC-UV）. All important variables influencing the extraction efficiency, such as pH, types of the extraction solvent and the disperser solvent and their volume, ionic strength and centrifugation time were investigated and optimized. Under the optimal conditions, the limit of detection （LODs） and quantification （LOQs） of the method were 13 and 39 ng/mL for CLZ, and 2 and 6 ng/mL for CPZ, respectively. The relative standard deviations （RSDs） of the targets were less than 5.1% （C=0.100 μg/mL, n=9）. Good linear behaviors over the tested concentration ranges were obtained with the values of R20.999 for the targets. The absolute extraction efficiencies of CLZ and CPZ from the spiked blank urine samples were 98.3% and 97.8%, respectively. The applicability of the technique was validated by analyzing urine samples and the mean recoveries for spiked urine samples ranged from 93.3% to 105.0%. The method was successfully applied for the determination of CLZ and CPZ in real human urine.展开更多
In this work, a novel flower-like cobalt-based metal organic frameworks(MOFs) self-assembled by Co^(2+) and nicotinic acid have been designed and synthesized. After a simple annealing treatment, Co_3O_4 nanoparticles ...In this work, a novel flower-like cobalt-based metal organic frameworks(MOFs) self-assembled by Co^(2+) and nicotinic acid have been designed and synthesized. After a simple annealing treatment, Co_3O_4 nanoparticles in-situ decorating on nitrogen doped graphite carbon-sheet(Co_3O_4/NC) were obtained. The resultant Co_3O_4/NC hybrid with unique flower-like structure and ration combination of Co_3O_4 nanoparticles and nitrogen doped graphite carbon, endowing the hybrid with enhanced electrical conductivity,short ion diffusion pathways and rich porosity to the materials, which can largely alleviate the problems of Co_3O_4 such as inferior intrinsic electrical conductivity, sluggish ion kinetics and large volume change upon cycling. When evaluated as anode material for sodium-ion batteries(SIBs), the Co_3O_4/NC hybrid exhibits satisfied reversible capacity(213.9 mAh g^(-1) after 100 cycles at 0.1 A g^(-1) ), excellent rate capability(145.4 m Ah g^(-1) at 2 A g^(-1) and 130.1 mAh g^(-1) at 4 A g^(-1) ) and robust long-term cycling stability(120.1 m Ah g^(-1) after 2000 cycles at 0.5 A g^(-1) ), showing great potential for high-performance SIBs.展开更多
Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 common peaks were analyzed, their average similarity was 97.29%. CFP were positioned with main index composition such as formononetin, calyco...Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 common peaks were analyzed, their average similarity was 97.29%. CFP were positioned with main index composition such as formononetin, calycosin and then the contents of index composition were determined. The character and exclusive of CFP of 10 samples of hongqi were clear. CFP and content determination of index composition of hongqi could be used to evaluate the quality of hongqi comprehensively.展开更多
Electrochemical properties of lithium-sulfur(Li-S)batteries are mainly hindered by both the insulating nature of elemental sulfur(i.e.,molecular S8)and the shuttling effect or sluggish redox kinetics of lithium polysu...Electrochemical properties of lithium-sulfur(Li-S)batteries are mainly hindered by both the insulating nature of elemental sulfur(i.e.,molecular S8)and the shuttling effect or sluggish redox kinetics of lithium polysulfide intermediates(Li_(2)S_(n),3≤n≤8).In this paper,a three-dimensional mesoporous reduced graphene oxide-based nanocomposite,with the embedding of metallic Co nanoparticles and the doping of elemental N(Co/NrGO),and its simply ground mixture with powdered S at a mass ratio of 1:6(Co/NrGO/S)are prepared and used as cathode-/separator-coated interlayers and working electrodes in assembled Li-S cells,respectively.One of the effective cell configurations is to paste composite Co/NrGO onto both the S-loading cathode and separator,showing good cycling stability(1070mAh g^(−1) in the 100th cycle at 0.2 C),highrate capability(835mAh g^(−1),2.0 C),and excellent durability(905mAh g^(−1) in the 250th cycle at 0.5 or 0.2 C).Compared with the experimental results of Co-absent NrGO,electrochemical properties of various Co/NrGO-based cell configurations clearly show multiple functions of Co/NrGO,indicating that the absence of Co/NrGO coatings and/or Co nanoparticles may be inadequate to achieve superior S availability of assembled Li-S batteries.展开更多
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the National Natural Science Foundation of China(No.22274021)Natural Science Foundation of Fujian Province(No.2022J01535)for financial support。
文摘Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morphology,good monodispersity and high specific surface area,were used as a stationary phase for high-performance liquid chromatography(HPLC).The single-crystal 3D COFs packed column not only exhibits high efficiency in separating hydrophobic molecules involving substituted benzenes,halogenated benzenes,halogenated nitrobenzenes,aromatic amines,aromatic hydrocarbons(PAHs)and phthalate esters(PAEs),but also achieves baseline separation of acenaphthene and acenaphthylene with similar physical and chemical properties as well as environmental pollutants,which cannot be quickly separated on commercial C18 column and a polycrystalline 3D COFs packed column.Especially,the column efficiency of 17303-24255 plates/m was obtained for PAEs,and the resolution values for acenaphthene and acenaphthylene,and carbamazepine(CBZ)and carbamazepine-10,11-epoxide(CBZEP)were 1.7and 2.2,respectively.This successful application not only confirmed the great potential of the singlecrystal 3D COFs in HPLC separation of the organic molecules,but also facilitates the application of COFs in separation science.
文摘High-entropy alloy(HEA)offer tunable composition and surface structures,enabling the creation of novel active sites that enhance catalytic performance in renewable energy application.However,the inherent surface complexity and tendency for elemental segregation,which results in discrepancies between bulk and surface compositions,pose challenges for direct investigation via density functional theory.To address this,Monte Carlo simulations combined with molecular dynamics were employed to model surface segregation across a broad range of elements,including Cu,Ag,Au,Pt,Pd,and Al.The analysis revealed a trend in surface segregation propensity following the order Ag>Au>Al>Cu>Pd>Pt.To capture the correlation between surface site characteristics and the free energy of multi-dentate CO_(2)reduction intermediates,a graph neural network was designed,where adsorbates were transformed into pseudo-atoms at their centers of mass.This model achieved mean absolute errors of 0.08–0.15 eV for the free energies of C_(2)intermediates,enabling precise site activity quantification.Results indicated that increasing the concentration of Cu,Ag,and Al significantly boosts activity for CO and C_(2)formation,whereas Au,Pd,and Pt exhibit negative effects.By screening stable composition space,promising HEA bulk compositions for CO,HCOOH,and C_(2)products were predicted,offering superior catalytic activity compared to pure Cu catalysts.
基金National Natural Science Foundation of China (Grant No.21372015 and 20872006)
文摘A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.
基金The Scholarship Supported by Ministry of Education of China for Research Abroad(No.3037[2006])the Excellent Doctoral Dissertation Foundation of Southeast University (No.YBTJ-0512)the National Basic Research Program of China(973Program)(No.2009CB623203)
文摘In order to investigate the effects of two mineral admixtures （i. e., fly ash and ground slag）on initial defects existing in concrete microstructures, a high-resolution X-ray micro-CT（ micro-focus computer tomography）is employed to quantitatively analyze the initial defects in four series of highperformance concrete （HPC）specimens with additions of different mineral admixtures. The nigh-resolution 3D images of microstructures and filtered defects are reconstructed by micro- CT software. The size distribution and volume fractions of initial defects are analyzed based on 3D and 2D micro-CT images. The analysis results are verified by experimental results of watersuction tests. The results show that the additions of mineral admixtures in concrete as cementitious materials greatly change the geometrical properties of the microstructures and the spatial features of defects by physical-chemistry actions of these mineral admixtures. This is the major cause of the differences between the mechanical behaviors of HPC with and without mineral admixtures when the water-to-binder ratio and the size distribution of aggregates are constant.
基金The National Natural Science Foundation of China(Grant No.81202918)the Open Project of National First-Class Key Discipline for Science of Chinese Materia Medica,Nanjing University of Chinese Medicine(Grant No.2011ZYX2-006)+2 种基金the Science and Technology Project of Hangzhou,China(Grant No.20130533B68 and 20131813A23)the Chinese Medicine Research Program of Zhejiang Province,China(Grant No.2014ZQ008 and 2015ZQ011)the Science Foundation of Zhejiang Chinese Medical University(Grant No.2011ZY25 and 2013ZZ12)
文摘The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs, a simple, easy, and sensitive high-performance liquid chromatography coupled with diode array detectors was developed for simultaneous determination of nine bioactive components in the herbal pairs. The calibration curve exhibited good linearity（r2≥0.9992）. The LODs and LOQs were ≤7.30 and 11.53 μg/m L, respectively. The intra-, inter-day and repeatability RSD values of the nine compounds were less than 3.86%, 2.71%, and 4.29%, respectively. The RSD stability values were less than 3.64%. The recovery of the method was in the range of 96.70%–102.10%, with RSD values less than 3.52%. The developed method can be applied to the intrinsic quality control of crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs.
文摘The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture of chloroform-n-heptane.2-(4-Hydrazinocarbonyl- phenyl)-4,5-diphenylimidazole (HCPI) was used as a fluorescent labelling reagent of the fatty acids. The labelling reaction was carried out at 30℃ for 1 h at pH 6.5 and the resulting reaction mixture was sudjected to HPLC. The labelled fatty acid C_(17)(P-C_(17))was used as the internal standard. The la- belled fatty acids C_(16) and C_(18) were separated within 18 min on an ODS-8OTM column (150 mm× 6 mm ID,5μm,Tosoh Japan).The calibrlation curves of fatty acids from the spiked control serum were Y_1=-0.003 7 + 0.0028X_1,r=0.994 for FA C_( 16) and Y_2=0.00 1 2 + 0.00098X_2,r=0.999 for FA C_( 18),respectively.The average recoveries of facids from the spiked contrl serum were 107.2%(n=8,RSD=4.3%)for FA C_(16) and 97.35%(n=8, RSD=4.0%)for FA C_(18),respectively.The lower detection limits of fatty acids after reaction were 12μmol per 20μl injection for FA C_(16) and 18 μmol per 20μl injection for FA C_(18),respectively(signal to noise ratio, S/N=2).The HPLC/CL method was applied to the determination of FA C_(16) and FA C_(18) in normal human serum and the results showed that the concentrations of fatty acids in normal human serum were 0.134 ± 0.009 μ mol/ml serum(n=5) for FA C_(16) and 0.052±0.028 μmol/ml serum(n=5)for FA C_(18),respectively.
基金Program for Changjiang Scholar and Innovative Team in University(Grant No.985-2-063-112)
文摘We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid （TFA） aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL （r2= 0.9998）, 9.38-1407 μg/mL （rz = 0.9999）, 80.6-8060μg/mL （r2 = 0.9999） and 2.10---630μg/mL （r2 = 0.9987） with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.
文摘Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-Aq column using a gradient elution with mobile phase of 8 mmol^L-1 ammonium acetate aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL·min^-1 at 25 ℃ with the diode-array detection at 260 nm. Results Cytidine, uridine, guanosine, adenosine and uracil had good linearity in the ranges of 1.79 - 57.40 μg·mL^-1 （r^2 = 1.0000）, 3.30 - 105.60 μg·mL^-1 （r^2 = 1.0000）, 3.09 - 98.80 μg·mL^ -1（r^2 = 0.9999）, 2.77 - 88.60 μg·mL^-1 （r^2 = 1.0000） and 0.38 - 12.30 μg·mL ^-1 （r^2 = 1.0000） with average recoveries of 93.9%, 96.5%, 92.7%, 93.2% and 98.8%, respectively. The content of cytidine, uridine, guanosine, adenosine and uracil in different parts of P. notogingeng were significantly different. Conclusion This is the first report on quantitative determination of nucleosides and nucleobases in P notoginseng.
文摘The compositions and contents of ginsenbsides in Panax ginseng,P.quinquefolium and P.notoginseng were determined and compared by reversed-phase High-Performance Liquid Chro- matography(HPLC).The method was performed on an Alltech Adsorbosphere HS C_(18) column,using 5×10^(-3)M NaH_2PO_4-H_3PO_4 buffer solution(pH 3.0)and acetonitrile-water(50:50)as gradient eluents. The baseline separation of ginsenosides Rb_1,Rb_2,Rb_1,Rc,Rd,Rf,Ro,and Re+Rg_1 was obtained in one analytical run.The ginsenosides are directly detected at 203 nm.The detection limit is 40μg at a signal to noise ratio of 3:1.The improved sample preparation and clean-up prior to injection with SEP-PAK C_(18)cartridge strongly reduced the front peaks caused by the impurities in the methanolic extracts of samples to afford a smooth baseline and clear background.The HPLC patterns of methanolic extracts mainly including the ginsenosides were found capable of serving as chemical fingerprints to differentiate the three species from each other.It was also found that there are no significant diffe- rences of the HPLC patterns between the wild Panax ginseng and the cultivated,the white and the red ginsengs,Chinese and Korean red ginsengs,and the tap roots of Panax ginseng collected in four consecutive months,only certain differences in contents of ginsenosides do exist.The contents of the nine major ginsenosides present in the rhizome,tap root and rootlet as well as the leaf of Panax quinquefolium were also determined and compared.
基金Supported by National Natural Science Foundation of China,Grant No.81360356Scientific Research Foundation of Xinjiang Medical University,Grant No.XJC201221
文摘AIM: To perform plasma free amino acid (PFAA) profiling of esophageal squamous cell carcinoma (ESCC) patients at different pathological stages and healthy subjects.
文摘The various advantages of organic polymer monoliths, including relatively simple preparation processes,abundant monomer availability, and a wide application range of pH, have attracted the attention of chromatographers. Organic polymer monoliths prepared by traditional methods only have macropores and mesopores, and micropores of less than 50 nm are not commonly available. These typical monoliths are suitable for the separation of biological macromolecules such as proteins and nucleic acids, but their ability to separate small molecular compounds is poor. In recent years, researchers have successfully modified polymer monoliths to achieve uniform compact pore structures. In particular, microporous materials with pores of 50 nm or less that can provide a large enough surface area are the key to the separation of small molecules. In this review, preparation methods of polymer monoliths for high-performance liquid chromatography, including ultra-high cross-linking technology, post-surface modification, and the addition of nanomaterials, are discussed. Modified monolithic columns have been used successfully to separate small molecules with obvious improvements in column efficiency.
基金Project (No. 2008BAI55B03) supported by the Key Project of the National Science and Technology Pillar Program, China
文摘A high-performance liquid chromatography （HPLC） system was used in the reversed phase mode for the determination ofbenzalkonium chloride （BKC） in azithromycin viscous ophthalmic drops. A Venusil-XBP（L）-C18 （150 mm×4.6 mm, 5 gm） column was used at 50℃. The mobile phase consisted of a mixture of methanol-potassium phosphate （16：5, v/v）. Two sample preparation methods were compared. The results suggested that, compared with an extraction procedure, a deproteinization procedure was much quicker and more convenient. Using the deproteinization procedure for sample preparation, calibration curves were linear in the range 5.0-50μg/ml. The within-day and inter-day coefficients of variation were less than 10%. The average recoveries were determined as 96.70%, 98.52%, and 97.96% at concentrations of 10.0, 30.0, and 50.0 μg/ml, respectively. Variability in precision did not exceed 5%. In conclusion, this HPLC method using a simple sample treatment procedure appears suitable for monitoring BKC content in azithromycin viscous ophthalmic drops.
基金Project supported by the National Natural Science Foundation of China(No.31430067)the Northeast Agricultural University Innovation Foundation for Postgraduate of Heilongjiang Province(No.yjscx14058)the National High-Tech R&D Program(863)of China(No.2013AA102104)
文摘Camellia seed oil （CSO） is rich in oleic acid and has a high number of active components, which give the oil high nutritional value and a variety of biological activity. The aim of the present study was to determine the changes in the content and distribution of total polar compounds （TPC） in CSO during heating. TPC were isolated by means of preparative flash chromatography and further analyzed by high-performance size-exclusion chromatography （HPSEC） The TPC content of CSO increased from 4.74% to 25.29%, showing a significantly lower formation rate as compared to that of extra virgin olive oil （EVOO） and soybean oil （SBO） during heating. Furthermore, heating also resulted in significant differences （P〈0.05） in the distribution of TPC among these oils. Though the content of oxidized triacyl- glycerol dimers, oxidized triacylglycerol oligomers, and oxidized triacylglycerol monomers significantly increased in all these oils, their increased percentages were much less in CSO than those in EVOO, indicating that CSO has a greater ability to resist oxidation. This work may be useful for the food oil industry and consumers in helping to choose the correct oil and to decide on the useful lifetime of the oil.
基金supported by the National Natural Science Foundation of China(No.21275088)
文摘Creatinine, uric acid, hypoxanthine and xanthine are important diagnostic biomarkers in human urine for gouty arthritis or renal disease diacrisis. A simple method for simultaneous determination of these biomarkers in urine based on reversed-phase high-performance liquid chromatography （RP-HPLC） with ultraviolet （UV） detector was proposed. After pretreatment by dilution, centrifugation and filtration, the biomarkers in urine samples were separated by ODS-BP column by elution with methanol/50 mM NaH2PO4 buffer solution at pH 5.26 （5：95）. Good linearity between peak areas and concentrations of standards was obtained for the biomarkers with correlation coefficients in the range of 0.9957-0.9993. The proposed analytical method has satisfactory repeatability （the recovery of data in a range of creatinine, uric acid, hypoxanthine and xanthine was 93.49-97.90%, 95.38-96.45%, 112.46-115.78%and 90.82-97.13%with standard deviation of o5%, respectively） and the limits of detection （LODs, S/N Z 3） for creatinine, uric acid, hypoxanthine, and xanthine were 0.010, 0.025, 0.050 and 0.025 mg/L, respectively. The established method was proved to be simple, accurate, sensitive and reliable for the quantitation of gouty arthritis＇ biomarkers in human urine samples. The ratio of creatinine to uric acid was found to be a possible factor for assessment of gouty arthritis.
文摘Aim A reliable high-performance liquid chromatographic (HPLC) method wasdeveloped for determination of germacrone in rat plasma. Methods The plasma samples were treatedwith acetonitrile and analyzed by HPLC with UV detection at 244 nm. Results The limit of detectionwas 100 ng·mL^(-1) for germacrone in plasma and the linear range was 0.1004-15.06 μg·mL^(-1) inplasma. The RSD of intra-day and inter-day assay was 1.87% - 4.29% and 1.29% -5.15%, respectively.The recoveries of germacrone were over 95%. The endogenous substances in plasma did not show anyinterference in the analysis. Conclusion The method is accurate and convenient, and suitable forpharmacokinetic studies of germacrone in rats.
基金supported by Science Research Funds of Medical Course, HUST
文摘A simple method has been proposed for the determination of clozapine （CLZ） and chlorpromazine （CPZ） in human urine by dispersive liquid-liquid microextraction （DLLME） in combination with high-performance liquid chromatography-ultraviolet detector （HPLC-UV）. All important variables influencing the extraction efficiency, such as pH, types of the extraction solvent and the disperser solvent and their volume, ionic strength and centrifugation time were investigated and optimized. Under the optimal conditions, the limit of detection （LODs） and quantification （LOQs） of the method were 13 and 39 ng/mL for CLZ, and 2 and 6 ng/mL for CPZ, respectively. The relative standard deviations （RSDs） of the targets were less than 5.1% （C=0.100 μg/mL, n=9）. Good linear behaviors over the tested concentration ranges were obtained with the values of R20.999 for the targets. The absolute extraction efficiencies of CLZ and CPZ from the spiked blank urine samples were 98.3% and 97.8%, respectively. The applicability of the technique was validated by analyzing urine samples and the mean recoveries for spiked urine samples ranged from 93.3% to 105.0%. The method was successfully applied for the determination of CLZ and CPZ in real human urine.
基金supported financially by the Anhui Provincial Key Research and Development Program(No.1704A0902022)the College Natural Science Key Foundation of Anhui Province(No.KJ2018A0453)+2 种基金the Innovative Research Team of Anhui Provincial Education Department(No.2016SCXPTTD)the Key Discipline of Material Science and Engineering of Suzhou University(No.2017XJZDXK3)the Key Scientific Research Projects of Suzhou University(No.2016yzd02)
文摘In this work, a novel flower-like cobalt-based metal organic frameworks(MOFs) self-assembled by Co^(2+) and nicotinic acid have been designed and synthesized. After a simple annealing treatment, Co_3O_4 nanoparticles in-situ decorating on nitrogen doped graphite carbon-sheet(Co_3O_4/NC) were obtained. The resultant Co_3O_4/NC hybrid with unique flower-like structure and ration combination of Co_3O_4 nanoparticles and nitrogen doped graphite carbon, endowing the hybrid with enhanced electrical conductivity,short ion diffusion pathways and rich porosity to the materials, which can largely alleviate the problems of Co_3O_4 such as inferior intrinsic electrical conductivity, sluggish ion kinetics and large volume change upon cycling. When evaluated as anode material for sodium-ion batteries(SIBs), the Co_3O_4/NC hybrid exhibits satisfied reversible capacity(213.9 mAh g^(-1) after 100 cycles at 0.1 A g^(-1) ), excellent rate capability(145.4 m Ah g^(-1) at 2 A g^(-1) and 130.1 mAh g^(-1) at 4 A g^(-1) ) and robust long-term cycling stability(120.1 m Ah g^(-1) after 2000 cycles at 0.5 A g^(-1) ), showing great potential for high-performance SIBs.
文摘Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 common peaks were analyzed, their average similarity was 97.29%. CFP were positioned with main index composition such as formononetin, calycosin and then the contents of index composition were determined. The character and exclusive of CFP of 10 samples of hongqi were clear. CFP and content determination of index composition of hongqi could be used to evaluate the quality of hongqi comprehensively.
基金The authors are grateful for the financial support of the National Natural Science Foundation of China(21673131)the Natural Science Foundation of Fujian Province(2019J01800).
文摘Electrochemical properties of lithium-sulfur(Li-S)batteries are mainly hindered by both the insulating nature of elemental sulfur(i.e.,molecular S8)and the shuttling effect or sluggish redox kinetics of lithium polysulfide intermediates(Li_(2)S_(n),3≤n≤8).In this paper,a three-dimensional mesoporous reduced graphene oxide-based nanocomposite,with the embedding of metallic Co nanoparticles and the doping of elemental N(Co/NrGO),and its simply ground mixture with powdered S at a mass ratio of 1:6(Co/NrGO/S)are prepared and used as cathode-/separator-coated interlayers and working electrodes in assembled Li-S cells,respectively.One of the effective cell configurations is to paste composite Co/NrGO onto both the S-loading cathode and separator,showing good cycling stability(1070mAh g^(−1) in the 100th cycle at 0.2 C),highrate capability(835mAh g^(−1),2.0 C),and excellent durability(905mAh g^(−1) in the 250th cycle at 0.5 or 0.2 C).Compared with the experimental results of Co-absent NrGO,electrochemical properties of various Co/NrGO-based cell configurations clearly show multiple functions of Co/NrGO,indicating that the absence of Co/NrGO coatings and/or Co nanoparticles may be inadequate to achieve superior S availability of assembled Li-S batteries.
