[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 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
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
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
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
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
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
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
In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been develo...In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been developed.This method is simple and practical,which allows direct generation of characteristic mass spectra from the HPTLC plates automatically with the application of in situ solvent desorption interface.The HPTLC silica gel plates were developed with toluene-ethyl formate-formic acid(5:5:0.2,V/V)and all bands were transferred to QDa system directly in situ using 80%methanol with 0.1%formic acid as desorption solvent.The acquired HPTLC-QDa spectra showed that luminous yellow band b3,containing ganoderic acid B/G/H and ganodeneric acid B,the major active components of Ganoderma,could be found only in G.lucidum and G.lucidum(Antler-shaped),but not in G.sinense and G.applanatum.Moreover,bands b13 and b14 with m/z 475/477 and m/z 475/491/495,respectively,could be detected in G.lucidum(Antler-shaped),but not in G.lucidum,thus allowing simple and robust authentication of G.lucidum with confused species.This method is proved to be simple,practical and reproducible,which can be extended to analyze other herbal medicines.展开更多
In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation...In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation of impurity profile in moxifloxacin （MOX） drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.展开更多
In this study, we selected adult normal pituitary gland tissues from six patients during operations for pituitary microadenomas via the transsphenoidal approach for extended normal pituitary tissue resection around th...In this study, we selected adult normal pituitary gland tissues from six patients during operations for pituitary microadenomas via the transsphenoidal approach for extended normal pituitary tissue resection around the tumor, and analyzed the protein expression of human normal pituitary using two-dimensional high-performance liquid chromatography combined with LTQ-Orbitrap mass spectrometry proteomics technology. The ten most highly expressed proteins in normal human pituitary were： alpha 3 type VI collagen isoform 5 precursor （abundance among tall pituitary proteins 1.30%）, fibrinogen beta chain preproprotein （0.99%）, vimentin （0.73%）, prolactin （0.69%）, ATP synthase, H~ transporting and mitochondrial F1 complex beta subunit precursor （0.52%）, keratin I （0.49%）, growth hormone （0.45%）, carbonic anhydrase I （0.40%）, heat shock protein 90 kDa I （0.31%）, and annexin V （0.30%）. Based on the biological function classifications of these proteins, the top three categories by content were neuroendocrine proteins （abundance among all pituitary proteins, 40.1%）, catalytic and metabolic proteins （28.3%）, and cell signal transduction proteins （9.8%）. Based on cell positioning classification, the top three categories were cell organelle （24.5%） membrane （20.8%）, and cytoplasm （13.0%）. Based on biological process classification, the top three categories of proteins are involved in physiological processes （42.9%）, cellular processes （40.4%）, and regulation of biological processes （9.1%）. Our experimental findings indicate that a protein expression profile database of normal human pituitary can be precisely and efficiently established by proteomics technology.展开更多
A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compo...A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.展开更多
Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tr...Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.展开更多
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 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.
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.
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.
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.
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.
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National Key R&D Program of China(Nos.2019YFC1711000 and 2018YFC1707900)the National Natural Science Foundation of China(No.8200140730)Qi-Huang Scholar of National Traditional Chinese Medicine Leading Talents Support Program(2018)。
文摘In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been developed.This method is simple and practical,which allows direct generation of characteristic mass spectra from the HPTLC plates automatically with the application of in situ solvent desorption interface.The HPTLC silica gel plates were developed with toluene-ethyl formate-formic acid(5:5:0.2,V/V)and all bands were transferred to QDa system directly in situ using 80%methanol with 0.1%formic acid as desorption solvent.The acquired HPTLC-QDa spectra showed that luminous yellow band b3,containing ganoderic acid B/G/H and ganodeneric acid B,the major active components of Ganoderma,could be found only in G.lucidum and G.lucidum(Antler-shaped),but not in G.sinense and G.applanatum.Moreover,bands b13 and b14 with m/z 475/477 and m/z 475/491/495,respectively,could be detected in G.lucidum(Antler-shaped),but not in G.lucidum,thus allowing simple and robust authentication of G.lucidum with confused species.This method is proved to be simple,practical and reproducible,which can be extended to analyze other herbal medicines.
基金the Ministry of Public Health of the People's Republic of China(No200802038) for financial support
文摘In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation of impurity profile in moxifloxacin （MOX） drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.
基金supported by the National NaturalScience Foundation of China, No. 81200890
文摘In this study, we selected adult normal pituitary gland tissues from six patients during operations for pituitary microadenomas via the transsphenoidal approach for extended normal pituitary tissue resection around the tumor, and analyzed the protein expression of human normal pituitary using two-dimensional high-performance liquid chromatography combined with LTQ-Orbitrap mass spectrometry proteomics technology. The ten most highly expressed proteins in normal human pituitary were： alpha 3 type VI collagen isoform 5 precursor （abundance among tall pituitary proteins 1.30%）, fibrinogen beta chain preproprotein （0.99%）, vimentin （0.73%）, prolactin （0.69%）, ATP synthase, H~ transporting and mitochondrial F1 complex beta subunit precursor （0.52%）, keratin I （0.49%）, growth hormone （0.45%）, carbonic anhydrase I （0.40%）, heat shock protein 90 kDa I （0.31%）, and annexin V （0.30%）. Based on the biological function classifications of these proteins, the top three categories by content were neuroendocrine proteins （abundance among all pituitary proteins, 40.1%）, catalytic and metabolic proteins （28.3%）, and cell signal transduction proteins （9.8%）. Based on cell positioning classification, the top three categories were cell organelle （24.5%） membrane （20.8%）, and cytoplasm （13.0%）. Based on biological process classification, the top three categories of proteins are involved in physiological processes （42.9%）, cellular processes （40.4%）, and regulation of biological processes （9.1%）. Our experimental findings indicate that a protein expression profile database of normal human pituitary can be precisely and efficiently established by proteomics technology.
文摘A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.
文摘Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.
