最新刊期
卷 39 ， 期 1 ， 2020
- 摘要：Surface assisted laser desorption/ionization mass spectrometry(SALDI-MS) is a technique using inorganic nanoparticles and nanostructure surface as matrixes to facilitate desorption/ionization of analytes.Due to its advantages of high sensitivity,high salt tolerance,easy operation,good reproducibility and high throughput,SALDI-MS has been widely applied in the fields of food safety,environment monitoring and life science,etc.The recent development of SALDI-MS matrixes such as metal and metal oxide nanoparticles,carbon based materials,silica based materials and metal organic frameworks etc.and their applications in biological detection are summarized in this review.Finally,further perspective for the development of the novel matrixes and their potential applications are proposed.关键词：surface assisted laser desorption/ionization mass spectrometry(SALDI-MS);matrix;biological detection;nanomaterial
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发布时间：2023-05-25 - 摘要：Metabolomics is a powerful tool for small molecule metabolites analysis,and it is playing a more and more important role in the precision medicine and translational medicine.Mass spectrometry(MS) coupled with different chromatographic modes have become the pillar technology platforms for metabolomics due to their high sensitivity,good selectivity,wide dynamic range and rich information.Innovations and developments of these analytical methods are the important prerequisites for wide applications of metabolomics in various fields.Advances of the analytical methods focused on liquid chromatography-mass spectrometry based metabolomics technique in the past five years are summarized in this review,and the existing problems and future perspectives of this technique are also discussed.81 references are cited.关键词：metabolomics;one dimensional chromatography;multi dimensional chromatography;liquid chromatography-mass spectrometry
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发布时间：2023-05-25 - 摘要：Lipids play important roles in a variety of critical biological processes.Therefore,significant research efforts have been devoted to the structural characterization and functional analysis of lipids.Although mass spectrometry(MS) has become one of the most common techniques for rapid and sensitive analysis of lipids,the structural characterization on lipids remains to be an analytical challenge.Aiming to solve this problem,an effective and widely adopted method was developed for localizing C‖C(s) in unsaturated lipids and quantifying lipid C‖C location isomers.Besides,this method could be readily coupled with shotgun lipidomics,liquid chromatography-mass spectrometry(LC-MS) and MS imaging,to achieve detailed lipid structural analysis on various types of biological samples.关键词：lipids;tandem mass spectrometry;photochemical derivatization;structural elucidation
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发布时间：2023-05-25 - 摘要：In this work,an orthogonal separation method was developed for the separation of lycopene isomers based on the combination of low temperature(L-T) C18 column and C30 column.As the temperature decreased to -20 ℃,the resolution for the separation of lycopene isomers on a normal C18 column was greatly improved.After investigating the relation of solubility and resolution,seven kinds of lycopene isomers were finally prepared by the orthogonal separation method with their purities all higher than 97%.The loading capacity and purification effect of the orthogonal method for lycopene were much higher than that of the method only based on L-T C18 or C30 column.Then,the obtained all trans lycopene were dissolved in walnuts oil,black seed oil,almonds oil,grape seed oil,pumpkin seed oil and peach kernel oil,respectively,and heated at 120 ℃ to study their isomerization.Grape seed oil was regarded as the most valuable solvent for developing lycopene product due to its highest cis/all trans ratio of lycopene isomers after heating.Finally,the stability of cis isomers at 4 ℃ in edible oils was investigated by taking walnut oil as the example.Both the isomerization and degradation of these isomers happened with the increase of storage time.All trans lycopene and(13Z)lycopene were found as the preferential conformations in walnut oil.The obtained results were expected to provide some beneficial information for the development of lycopene product.关键词：lycopene;low temperature preparation;isomerization;degradation;edible oils
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发布时间：2023-05-25 - 摘要：Mass spectrometry imaging(MSI) as a novel molecules imaging technique,has made itself a powerful tool in biology and medicine research due to its inherent advantages of label free,simple sample preparation,and high throughput analysis.Ionization technology is the key and core of MSI.The development of novel ionization sources has greatly promoted the MSI applications.The principles and characteristics of current major MSI methods are mainly focused in this paper.Meanwhile,the MSI applications in tumor pathological diagnosis,biomarkers and drugs development are reviewed,and a reference for tumor clinical diagnosis is provided.关键词：mass spectrometry imaging;ion source;tumor;biomarker;drug
- 2030
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发布时间：2023-05-25 - 摘要：In addition to the canonical nucleobases,nucleic acids(DNA and RNA) carry a variety of chemical modifications.More than 150 chemical modifications so far have been identified in nucleic acids.These chemical modifications do not change the sequence of nucleic acids,but may alter their structures and biochemical properties,ultimately regulating the spatiotemporal expression of genes.Uncovering the functions of these modifications could promote our understanding of the physiological regulation mechanisms of living organisms.However,the abundance of nucleic acid modifications is usually low in vivo.Therefore,highly sensitive and specific detection methods are critical to decipher the functions of nucleic acid modifications.Chemical derivatization in combination with mass spectrometry techniques demonstrate to have excellent analytical capabilities for endogenous low abundance nucleic acid modifications.In the past few years,researchers have established a variety of chemical derivatization mass spectrometry based methods for sensitive and efficient analysis of nucleic acid modifications.The recent advances in deciphering nucleic acid modifications by chemical derivatization mass spectrometry are summarized in this review,and further promotion on the future studies of nucleic acid modifications is anticipated.关键词：chemical derivatization;mass spectrometry analysis;epigenetics;nucleic acid modifications;clinical samples
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发布时间：2023-05-25 - 摘要：Aiming at the current situation of long time and cumbersome operation in precise screening of macroporous resins with high selective separation performance for polysaccharides of traditional Chinese medicine,a predictive model for the rapid screening of macroporous resins was constructed in this paper.A multi source information model for the parameters of a macroporous adsorption resin,the molecular weight of glucan and the adsorption capacity was established by using R language,which was used to quickly predict and screen the type of macroporous adsorption resin with the optimal adsorption effect for polysaccharides of traditional Chinese medicine.The correlation coefficient(r2) of the established multi source information model is 0.901 2,the P value is 0.000 782 and the root mean square error(RMSE) is 19.89,which was verified with lycium barbarum polysaccharide,and was used to predict the adsorption effects of LX-T19,LX-T81,LX-20,LX-1180 and D101 type macroporous adsorption resins on lycium barbarum polysaccharides.Results showed that LX-20 is the best macroporous adsorption resin,with its adsorption capacity of 117.40 mg·g-1,while its actual adsorption capacity by the verification experiment is 111.23 mg·g-1.The established multi source information prediction model is accurate and reliable,and has a reference value for the precise and rapid screening of macroporous adsorption resins used for purification of polysaccharides in Chinese medicine.关键词：macroporous adsorption resin;glucan;R language;multi source information model
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发布时间：2023-05-25 - 摘要：To study the quality markers of Danhe granule for treatment of hyperlipidemia,the network of “hyperlipidemia-common target-components of Danhe granules in vivo” was constructed by Cytoscape software based on the results of in vivo component analysis.To determine the key target and component,the biological process,pathway enrichment and network topology of the common target were analyzed by DAVID and String database,respectively.Then HepG2 cells induced by oleic acid(OA) were selected to establish a lipid accumulation cell model to verify the lipid-lowering efficacy of the key components.Finally,combined with the content,stability and characteristics of the related components in the preparation,the quality markers were determined.Result showed that components of Danhe granule in vivo act on 10 disease targets of hyperlipidemia,including CES1,ADORA2A,ADORA1,APOB,LDLR,PPARA,PPARG,INSR,ESR2 and ESR1,which mainly regulated the process of lipid metabolism and the signal pathways of PPAR and cAMP.It was found that LDLR,PPARA and PPARG may be the key targets for the lipid-lowering effect of Danhe granules,while the components interacted with the key targets were resveratrol and naringenin.Futhermore,resveratrol or naringenin could not only reduce the number of intracellular lipid droplets,improve the severity of lipid accumulation in HepG2 cells,but also significantly reduce the content of intracellular triglyceride which may be the key components.Considering that the resveratrol and naringenin in vivo come from polydatin and naringin in preparation,while polydatin and naringin are rich and stable in preparation with obvious characteristics,they thus could be used as the quality markers of Danhe granules in the treatment of hyperlipidemia.This study provides a reasonable candidate quality control index for the establishment of the quality standard of Danhe granules.关键词：Danhe granules;quality marker;quality control index;network pharmacology;hyperlipidemia
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发布时间：2023-05-25 - 摘要：Stroke is one of the leading causes for death and disability in the world,while ischemic stroke(IS) constitutes around 87 percent of stroke cases.Medical treatment should typically be made within 3 or 45 hours of stroke onset.Rapid diagnosis and early screening on IS are thus of great significance,and molecular biomarker is an effective strategy for this.Mass spectrometry is a choice of technique for detection of various compounds in biomedical samples,and has played important roles in discovery of biomarkers for IS.In this review,the recent advances in discovering biomarkers of IS,particularly those of the protein and metabolite biomarkers,are summarized and commented.关键词：mass spectrometry;ischemic stroke;biomarkers;proteins;metabolites
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发布时间：2023-05-25 - 摘要：As a traditional prescription of Tibetan drug,Sanweidoukou decoction could be made from boiling herbal medicine cardamom,cumin,piper longum with yak milk together.It is reported to possess therapeutic efficacies against various diseases including Alzheimer′s disease(AD).However,its composition is still unclear due to its complex constituents with different polarities and volatilities.The principal objective of this research is to investigate the chemical constituents of the decoction.Considering different physicochemical properties of various components,gas chromatography tandem mass spectrometry(GC-MS) and ultra performance liquid chromatography coupled with high resolution mass spectrometry(UPLC-HRMS/MS) analysis were performed.As a result,99 compounds were identified and confirmed as monoterpenes or oxygenated monoterpenes from cardamom and cumin,such as eucalyptol,and alkaloids from piper longum such as piperine,as well as lipids from yak milk like triglycerides,etc.The results obtained provide a good support for further insight into Sanweidoukou decoctions pharmacological mechanism study in AD treatment.关键词：Sanweidoukou decoction;Alzheimer′s disease;gas chromatography mass spectrometry(GC-MS);ultra performance liquid chromatography coupled with high resolution tandem mass spectrometry(UPLC-HRMS/MS);chemical composition
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发布时间：2023-05-25 - 摘要：Ambient ionization mass spectrometry(AIMS) is a mass spectrometric technique developed for desorbing and ionizing samples under open-air environment，which requires no or minimal sample preparation.Along with the development of this family of techniques，applications of AIMS in clinical research have gained popularity in the past years.In this review，AIMS techniques employed in tumor diagnosis are discussed and summarized，and their futures are also envisioned.关键词：ambient ionization mass spectrometry;tumor;diagnosis
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发布时间：2023-05-25 - 摘要：A rapid method was established for the nondestructive determination of multi marker components in Aconiti Lateralis Radix Praeparata by near infrared spectroscopy(NIRS) combined with partial least squares(PLS) and least square-support vetor machine(LS-SVM).A total of 38 batches of samples were selected for the determination of six alkaloids,ie.benzoylmesaconine,benzoylaconine,benzoylhypaconine,meaconitine,hypaconitine and aconitin in Aconiti Lateralis Radix Praeparata by high performance liquid chromatography(HPLC),and their NIR spectra were further collected.Two determination calibration models between the six components and NIRS were established by PLS and LS-SVM methods,respectively.The relative prediction deviations(RPDs) for the six components the total of monoester type alkaloids and the total of diester type alkaloid were 3.3,3.2,4.1,7.7,8.8,7.6,4.0 and 8.6,while the rpre for the 8 types were 0.948 6,0.947 5,0.966 8,0.990 9,0.994 6,0.996 9,0.966 9 and 0.992 7,respectively.Results showed that the LS-SVM model was better than PLS model,indicating that a good nonlinear relation existed between the predicted values of NIRS model and the measured values of HPLC.The established NIRS combined with LS-SVM could be applied to the rapid determination of six alkaloids in Aconiti Lateralis Radix Praeparata,and even to the prediction of the total of monoester type alkaloids and the total of diester type alkaloid,which is beneficial for the quality control of the Aconiti Lateralis Radix Praeparata.关键词：near infrared spectroscopy(NIRS);Aconiti Lateralis Radix Praeparata;least square-support vetor machine(LS-SVM);partial least squares(PLS);monoester type alkaloids;diester type alkaloids附子(Aconiti Lateralis Radix Praeparata)
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发布时间：2023-05-25 - 摘要：Proteins are the workhorses of cells,their biological functions are regulated by their dynamic structures,interactions with other biomolecules and many other factors.Gaining detailed structural information of proteins or protein complexes is crucial to decipher the molecular mechanisms of important biological processes.Hydrogen deuterium exchange mass spectrometry(HDX-MS) is not only a powerful tool for studying the dynamic changes of protein structures and protein ligand/protein interactions,but also an important complement to traditional biophysical approaches.In this review,the basic principles,mechanism,experimental methods and recent development of HDX-MS are presented,especially focusing on its applications in protein dynamics,protein-small molecule interactions and protein-protein interactions.关键词：protein dynamics;protein-small molecule interactions;protein-protein interactions;hydrogen deuterium exchange mass spectrometry
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发布时间：2023-05-25 - 摘要：The near infrared spectra for the outer skin and inner capsule of citri reticulatae pericarpium from different habitats were collected.Different spectral pretreatment methods were used and the best method was selected. The identification model of citri reticulatae pericarpium origin was established by principal component analysis.It was found that there were obvious baseline drift and background interference in the raw spectra.The interferences could be eliminated to a certain extent by using single spectral pretreatment method.After using pretreatments of standard normal variate transform,multivariate scattering correction,first derivative,second derivative and continuous wavelet transform,the best identification results for the inner capsule data could be obtained,with an accuracy of 91.67%,while the optimal identification results for the outer skin data could be obtained by the maximum and minimum normalization pretreatment with an accuracy of 70.83%.A 100% of identification accuracy could be obtained by 9 combinations of two pretreatment methods for the outer skin data,and the optimal pretreatment combination for the inner capsule data was de-trending+maximum-minimum normalization,with an accuracy of 95.83%.However,the accuracies for three pretreatment combinations were lower than those for two pretreatment combinations,which indicated that useful information might be deducted if too many kinds of pretreatments were used.Results showed the nondestructive identification on citri reticulatae pericarpium of different origins could be achieved based on the combination of near infrared spectroscopy and spectral pretreatments,in which a 100% accuracy could be realized by using the outer skin data to optimizing combination of spectral pretreatment.关键词：Citri reticulatae Pericarpium;near infrared spectroscopy technology;optimized spectral pretreatments;principal component analysis
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发布时间：2023-05-25 - 摘要：Enzymes as biocatalysts,participate in many physiological processes,which are important biomarkers.The activity analysis of enzymes is of great significance for diagnosis and treatment of many diseases.Matrix assisted laser desorption ionization time of flight mass spectrometry(MALDI-TOF MS) has been widely used in various omics studies and biological molecules detections because of its good performances in sensitivity,throughput,speed and operation.It also has played an important role in enzymes activity analysis.The methods of MALDI-TOF MS for enzyme activity analysis and drug screening are reviewed in this paper,the merits and disadvantages of each method are discussed,the problems and challenges existed are put forward,and finally the perspectives for MALDI-TOF MS in enzyme activity analysis are outlooked.关键词：MALDI-TOF MS;enzymes activity;homogeneous;heterogeneous
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发布时间：2023-05-25 - 摘要：A fingerprint analysis method was developed for the quality control of Citrus aurantium by high performance liquid chromatography(HPLC).The separation was carried out on a Waters Tnature-ACCHROM C18(4.6 mm×250 mm,5 μm) column,using acetonitrile-05% formic acid water as mobile phase by gradient elution,and the common peaks in the fingerprint of Citrus aurantium were identified by high performance liquid chromatography-quadrupole time of flight-mass spectrometry(HPLC-QTOF-MS).Similaritity evaluation,cluster analysis(CA) ,principal component analysis(PCA) and orthogonal partial least square discriminant analysis(OPLS-DA) were used for the data analysis and quality evaluation on 22 batches of Citrus aurantium.Results showed that 12 common peaks were defined by the fingerprint,and 11 components were identified by HPLC-QTOF-MS.The similarities for 22 batches of Citrus aurantium samples were more than 0.9.The results obtained from CA,PCA and OPLS-DA were consistent,among which,the samples from Jiangxi Province were clustered into one group,while the samples from Hunan Province and Fujian Province were clustered into another group,and three quality differential markers were screened out as hesperidin,neohesperidin and naringin by OPLS-DA.The HPLC fingerprint for Citrus aurantium is stable and reliable,and could be used to provide a reference for its quality control.关键词：citrus aurantium;chromatographic fingerprint;cluster analysis(CA);principal component analysis(PCA);orthogonal partial least square discriminant analysis(OPLS-DA)
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发布时间：2023-05-25 - 摘要：Formalin fixed and paraffin embedding(FFPE) is the most commonly used technique for clinical tissue preservation，while FFPE tissues have the characteristics including standardized preparation process，easy to store，large sample quantity and retrospective clinical information，which make them the high quality library for biomarker discovery and verification.In recent years，a series of proteomics approaches have been developed，covering sample preparation，protein digesting，peptide separation and identification by mass spectrometry.The whole processes have the characteristics of micro scale sample quality，high sensitivity and high throughput.These methods have been successfully used in clinical proteomics researches，for example，the tumor precision medicine.The proteomics methods for FFPE tissue samples and their applications in oncobioloby are summarizd in this review，providing a valuable reference for proteomics based clinical precision medicine researches.关键词：formalin fixed and paraffin embedding(FFPE);clinical proteomics;cross linking;biomarker
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发布时间：2023-05-25 - 摘要：This study introduced the three parameters of comprehensive linear qualitative similarity Sl, comprehensive linear quantitative similarity Pl% and fingerprint variation coefficient α to establish a novel method comprehensive linear fingerprinting method(CLFM),which comprehensively evaluated the overall quality of traditional Chinese medicine from a qualitative and quantitative perspective.The fingerprints for Tuire Jiedu injection(TJI) samples at 210,254,265,330 and 360 nm wavelengths were collected by high performance liquid chromatography with diode array detection(HPLC/DAD),and followed by the data fusion.Meanwhile,four index components,including chlorogenic acid(CHA),forsythin A(FA),paeonol(PA) and saikosaponin D(SD) were quantitatively analyzed.The quality of the samples was identified by CLFM.Results showed that 10 batches of injection samples were divided into 5 levels,and 10 batches of intermediate samples were divided into 4 levels.The quantitative analysis results of the four index components were highly correlated with the quantitative similarity Pl% of the fingerprint,indicating that the CLFM could be used to replace the standard substance for sample quantitative analysis.This method provides a new idea for the overall quality control of traditional Chinese medicine.关键词：comprehensive linear quantitative fingerprinting method;Tuire Jiedu injection;multi component quantification;multi wavelength fusion method
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发布时间：2023-05-25 - 摘要：Protein carbonylation,an irreversible post translational modification,is closely related to many diseases and aging.The analysis of protein carbonylation is a challenge due to its low abundance,low ionization efficiency and relative chemical instability.Advances in mass spectrometry based proteomics have made it possible to conduct large scale studies on protein carbonylation,providing in turn the data support for the study of related regulatory pathways of protein carbonylation.The concept,pathways and analysis methods of protein carbonylation are presented in this review,and the advances in proteomic analysis of protein carbonylation are highlighted.关键词：oxidative stress;protein carbonylation;proteomics
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发布时间：2023-05-25 - 摘要：A high coverage matrix assisted laser desorption/ionization mass spectrometry imaging(MALDI-MSI) method was developed to visualize the spatial locations of a wide spectrum of metabolites in lotus seed in this paper，in which the spatial locations of alkaloids，flavonoids，amino acids，fatty acids，organic acids,cholines and phospholipids in lotus seed were successfully imaged.Results suggested that the alkaloids are mainly distributed in the lotus seed germ，the flavones are mainly located in the lotus seed germ and lotus seed skin，the levels of amino acids in lotus seed cotyledon are significantly higher than that in the lotus seed embryo，there are few distribution differences of fatty acids in different tissues of lotus seed，the levels of choline in the lotus seed germ and the bottom of the lotus seed cotyledon are higher than those in other tissue regions，glycerophosphocholine mainly distributes in the apex of the lotus seed cotyledon，and the levels of organic acids and most phospholipids in the lotus seed cotyledon are higher than that in the lotus seed embryo.This study provides a new way to investigate the drug quality and the metabolic networks of lotus seed.关键词：lotus seed;metabolites;matrix assisted laser desorption/ionization mass spectrometry imaging(MALDI-MSI);tissue distribution
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发布时间：2023-05-25 - 摘要：A novel method of digital chromatography-mass spectrometry fingerprints of agarwood was established by high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry(HPLC-Q-TOF-MS).The agarwood sample was ultrasonically extracted with ethanol,then determined by HPLC-Q-TOF-MS,thus high performance liquid chromatography-ultraviolet(HPLC-UV) chromatograms and total ion chromatograms of high resolution time of flight mass spectrometry(TOF-MS) could be obtained simultaneously.Establishment of the digital fingerprints was conducted by acquiring the exact mass number of each peak combined with retention time in the chromatogram,so as to obtain the unique digital information of each peak and characterize its chemical composition in digital form,and finally deduce its molecular formula by exact mass and isotopes.A total of 30 components were identified by secondary mass spectrometry and literature data.The method could provide the digital information similar to identification for each chemical component of agarwood.The compositions of agarwood could be fully acquired as the digital information is unique,and it provides scientific data for the researches on pharmacology,pharmacodynamics and quality specification of agarwood.关键词：high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry;agarwood;digital chromatography and mass spectrometry fingerprints
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发布时间：2023-05-25 - 摘要：In this paper，a chemiluminescence aptasensor for the highly sensitive detection of aflatoxin B1 (AFB1) was constructed based on the strategy of enzyme assisted target recycling amplification.The label free aptamer probe H1-S1 and hairpin probe H2 were well designed using G-quadruplex/hemin DNAzyme as the signal molecule.The aptamer probe bound to the target AFB1，which triggered the target recycling amplification reaction with the help of exonuclease I to generate hairpin H1.The hairpin H1 was hybridized with H2，releasing the complete G-quadruplex sequence.The G quadruplex sequence combined with hemin to form G quadruplex/hemin DNAzyme，which catalyzed the oxidation of luminol-H2O2 chemiluminescence system to generate chemiluminescence signals to achieve the amplified detection of AFB1.Under the optimal experimental conditions，the chemiluminescence intensity exhibited a good linear relationship(r2=0.995 5) with the logarithm of AFB1 concentration in the range of 0.001-100 ng/mL.The detection limit was 0.93 pg/mL，and the recoveries were in the range of 93.7%-107%.With the advantages of simple operation，high sensitivity and good specificity，this aptasensor has a good application prospect in the detection of aflatoxin contamination.关键词：aflatoxin B1(AFB1);chemiluminescence;target recycling;G quadruplex;DNAzyme;traditional Chinese medicine
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发布时间：2023-05-25 - 摘要：Three dammarane types of saponins,including notoginsenoside R1,Rd and 20(S)-Rg3 were transformed using dodeca phosphotungstic acid.The chemical structures and transformation pathways of their products were analyzed by high performance liquid chromatography coupled with electrospray ionization multi stage mass spectrometry(HPLC-ESI-MSn).Totally,protopanaxatriol type saponin R1 was transformed into nine products,ie.20(S)-25-OH-R2,20(R)-25-OH-R2,25-OH-T5,20(S)-R2,20(R)-R2,20(S)-25-epoxy-R2,20(R)-25-epoxy-R2,T5 and 3β,12β dihydroxy 6α (2 O β D xylopyranosyl β D glucopyranosyloxy) dammar-20(22),24 diene,while ten identical products were obtained from protopanaxadiol type saponin Rd and 20(S)-Rg3,including 20(S)-25-OH-Rg3,20(R)-25-OH-Rg3,25-OH-Rk1,25-OH-Rg5,20(S)-Rg3,20(R)-Rg3,(20S,25)-epoxy-Rg3,(20R,25)-epoxy-Rg3,Rk1 and Rg5.Based on the structural identification,the relative content variations of major products with the reaction time were determined,and the transformation pathways for dammarane type saponin in acid solution were sequentially summarized.Results showed that dammarane type saponin could be readily transformed into rare ginsenosides via deglycosylation and epimerization reaction at C20 position,followed by hydration,dehydration and cyclization reactions on the olefin chain of dammarane type aglycone.关键词：ginseng;dammarane type saponin;chemical transformation;HPLC-ESI-MSn
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发布时间：2023-05-25 - 摘要：A metabolomics method based on high performance liquid chromatography-ultrahigh resolution mass spectrometry was developed for the analysis of metabolites in kidney tissues.In order to achieve this goal,rat kidney tissues were ground into powder in liquid nitrogen,and extracted with a methyl tert butyl ether/methanol/water solvent system to obtain high polarity(lower layer) and low polarity(upper layer) extracts,respectively.Then,the high polarity and low polarity extracts were subjected to gradient elution separation on a hydrophilic HILIC column and a reversed phase C18 column,respectively,and subsequently detected by ultrahigh resolution mass spectrometry(Orbitrap Fusion Lumos).The mass spectrometry analysis was performed using an electrospray ionization(ESI) source operated in positive and negative ion mode with a scanning range of 100-1 000 Da and a mass resolution of 120 000.Results showed that with high sensitivity,high specificity and good stability,the proposed method could be used to obtain the comprehensive information of high polarity and low polarity metabolites in kidney tissues,providing a novel approach discovering new biomarkers for kidney disease and drug nephrotoxicity.关键词：high performance liquid chromatography-ultrahigh resolution mass spectrometry;metabolomics;kidney;sample preparation
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发布时间：2023-05-25 - 摘要：A method of ultra high performance liquid chromatography（UPLC） was developed for the quantitative determination of 10 active components in Yinlai decoction,which was subsequently used for the quality evaluation of Yinlai decoction.The chromatographic separation was performed on a Waters ACQUITY UPLC HSS T3 column（2.1 mm×100 mm,1.8 μm） by gradient elution with 0.1% formic acid water and 0.1% formic acid acetonitrile as mobile phases.The detection wavelength was firstly set at 320 nm for neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,sinapine thiocyanate,forsythoside I in the first 10 min,then switched to 350 nm for forsythoside A,quercitrin from 10 to 16 min,and finally switched to 320 nm for baicalin,oroxylin A-7-O-β-D-glucuronide,wogonoside from 16 to 30 min.Results showed that the method completed the baseline separation for 10 active components in Yinlai decoction within 30 min.There were good linear relationships for 10 components in the certain concentration ranges with their correlation coefficients（r） not less than 0.999 2.The limits of detection and limits of quantitation were in the ranges of 0.018 8-0.075 0 μg·mL-1 and 0.062 5-0.250 μg·mL-1,respectively.The content range for 10 components ranged from 0.204 to 38.129 mg·g-1,in which baicalin was the highest,while quercitrin was the lowest.The method was used in the detection of three batches of sample,and it was found that the contents of the measured components were stable and consistent.The established analytical indexes are relatively comprehensive,reasonable and feasible,and could be used for better characterization and evaluation of the quality of Yinlai decoction.关键词：Yinlai decoction;ultra high performance liquid chromatography;wavelengths switching;quantitative analysis;quality evaluation
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发布时间：2023-05-25 - 摘要：A method of ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of 16 flavonoid glycosides and 4 terpenoid lactones in shuxuening injections.The samples were firstly diluted with methanol water(1%1,by volume),and then separated on an ACQUITY UPLC BEH Shield RP18 column(17 μm,21 mm×100 mm) by gradient elution using acetonitrile-water containing 01% formic acid as mobile phases,finally detected by UPLC-MS/MS with ESI source in MRM mode.Results revealed that the 20 compounds could be analyzed within 10 min.There were good linear relationships for twenty compounds in a certain concentration range with their correlation coefficients(r2) no less than 0963 3.The limits of detection(LODs) and limits of quantitation(LOQs) were in the ranges of 002-159 ng/mL and 007-530 ng/mL,respectively.And the recoveries at three levels were between 859-109%.This method was applied in the simultaneous detection of 16 flavonoid glycosides and 4 terpenoid lactones in different shuxuening injection products.With the advantages of simplicity,rapidness and good repeatability,the method is suitable for the quantitative analysis of 20 compounds in shuxuening injections,and provides a good strategy for further quality control of shuxuening injections.关键词：shuxuening injection;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);flavonoid glycosides;terpenoid lactones;simultaneous quantitative analysis
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发布时间：2023-05-25 - 摘要：Molecular weight determination and glycoform identification are the essential characterization data in stages ranged from development to quality control of therapeutic monoclonal antibodies(mAbs)，while determinations on mAbs at the intact protein level have been demonstrated to provide straightforward and valid data，which require instruments with high resolving power and involve sophisticated parameter settings.To reduce possible artifacts，impacts of parameters were investigated，including nominal resolution，in source fragmentation，collision induced dissociation and solution composition on the molecular weight determination and glycoform identification of intact Abs by orbitrap mass spectrometry with nanospray ionization in native mass spectrometric mode，so as to provide a useful reference for this kind of mass spectrometric analysis.关键词：monoclonal antibody;native mass spectrometry;intact protein;post translational modification;glycoform
- 1961
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- 4
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- 1
发布时间：2023-05-25 - 摘要：A urinary metabonomics method based on ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry(UHPLC-Q-TOF MS) was established for the investigation on mechanism of Radix Scutellariae-Gardenia jasminoides couples treating diabetic nephropathy.A diabetic model was established by streptozotocin intraperitoneal injection and feeding with high fat and high sucrose chow.After intragastric administration for 12 weeks,UHPLC-Q-TOF MS was used to analyze the metabolic profiles of the urinary samples from the control group,the model group and the Radix Scutellariae-Gardenia jasminoides Couples treatment group,which were then compared with the results from the Radix Scutellariae treatment group and the Gardenia jasminoides treatment group.The data were analyzed by Orthogonal partial least-squares discriminant analysis(OPLS-DA).According to the results of OPLS-DA，the compounds providing greater contribution to separation of each group were searched from the HMDB databases.Finally,31 potential biomarkers were identified,and 16 of them were related to the RadixScutellariae-Gardenia jasminoides Couples.Results revealed that Radix Scutellariae-Gardenia jasminoides couples played a role in diabetic nephropathy treatment through mainly affecting the pathways of tryptophan metabolism,phenylalanine metabolism,tyrosine metabolism,energy metabolism and biosynthesis of bile acids,in which biosynthesis of bile acids,urotoxin metabolism and energy metabolism are the important pathways to treat diabetic nephropathy.Compared with the single drug of Radix Scutellariae or Gardenia jasminoides,Radix Scutellariae-Gardenia jasminoides couples had the special treatment effect.关键词：Radix Scutellariae-Gardenia jasminoides couples;Radix Scutellariae;Gardenia jasminoides;diabetic nephropathy;urine
- 1955
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- 4
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- 3
发布时间：2023-05-25 - 摘要：A gold nanoparticles enhanced low temperature plasma ionization mass spectrometry was developed for the rapid determination of aniline.As an ambient mass spectrometry ion source,low temperature plasma(LTP) could meet the requirements for in situ and rapid detection.However,the matrix effect of water sample makes the detection sensitivity inadequate.In this study,low temperature plasma ion source was combined with gold nanoparticles modified acupuncture needles to create a good enhancement effect toward the mass spectrometry signal,which could be used to quickly and sensitively detect aniline.Results showed that the signal intensity for aniline is 56 times stronger.Meanwhile,the background noise is lower.There is a linear relationship between the signal intensity and the concentration of aniline in the range of 1-50 μg/L,with a detection limit(LOD) of 064 μg/L,and the consuming time for each sample is about 1 min.The proposed method herein is simple and easy to operate,and is expected to be applied in the detection of aniline in environmental water.关键词：aniline;low temperature plasma mass spectrometry;acupuncture needle;gold nanoparticles
- 1938
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- 4
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发布时间：2023-05-25 - 摘要：A novel paper spray ionization mass spectrometric(PSI-MS) method was developed for the direct detection of biofluid.The agarose hydrogel coated paper substrate was used to alleviate the lateral diffusion of polar extraction solvent to achieve both high extraction efficiency and ambient ionization,whereupon liquid-liquid extraction occurred between the biofluid sample droplet and the polar extract/spray solvent.Hence,the overall sensitivity of hydrogel coated PSI-MS could be improved greatly due to better extraction efficiency.Meanwhile,the evaporation rate for the extract/spray solvent was reduced due to its less diffusion,and a longer and more stable continuous mass spectrometry signal was obtained.In addition,ethyl acetate was used here as spray and extract solvents to form liquid-liquid extraction,high voltage DC was applied on the hydrogel coated paper substrate where sample was placed to achieve fast and accurate quantification of low abundance therapeutic drugs in biofluid samples.Compared with PSI-MS,the hydrogel coated PSI-MS extended the spray time by nearly 10 times and the signal for analyte by about 100 times.The method was applied in the quantitative detection of drugs in whole blood and urine samples with the limits of detection(LODs) decreased by 7-33 times.The hydrogel coated PSI-MS showed its great potential in the area of on site clinical diagnosis,owing to its simple preparation,high sensitivity and convenient operation.关键词：mass spectrometry;paper spray;liquid-liquid extraction;agarose hydrogel
- 2009
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- 4
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- 1
发布时间：2023-05-25 - 摘要：A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was established for the determination of five androgens,ie. dehydroepiandrosterone sulfate(DHEAS),androstenedione(A4),testosterone(T),17 hydroxyprogesterone(17 OHP) and dihydrotestosterone(DHT),in serum.The serum samples were extracted by solid phase extraction after protein precipitation,then separated on an Agela Venusil MP C18 column(30 mm×50 mm,3 μm) by gradient elution using methanol containing 01% formic acid and water with 002% formic acid as mobile phases,finally detected with electrospray ionization in positive or negative mode under multiple reaction monitoring(MRM) mode.As a result,there were good linear relationships for five androgens in their respective mass concentration ranges with correlation coefficients(r2) more than 0995,and the recoveries ranged from 960% to 105%.The intra and inter assay precision values for all androgens were less than 10%.The limits of quantitation for DHEAS,A4,T,17 OHP and DHT were 500,005,005,0025,0025 ng/mL,respectively.The method is rapid,accurate and sensitive,and could satisfy the requirements for clinical determination of serum androgens in patients with polycystic ovary syndrome(PCOS).关键词：polycystic ovary syndrome(PCOS);liquid chromatography-tandem mass spectrometry(LC-MS/MS);dehydroepiandrosterone sulfate(DHEAS);androstenedione(A4);testosterone(T);17 hydroxyprogesterone(17 OHP);dihydrotestosterone(DHT)
- 1819
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- 4
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- 2
发布时间：2023-05-25 - 摘要：Based on the advantages of ambient mass spectrometry in the fast and direct detection on samples without any pre treatment,an ambient mass spectrometric method was developed for the rapid and direct detection of drug tablets.In the experiment,a home made desorption electrospray ionization(DESI) device was fabricated for the fast mass spectrometry(MS) detection of commercial paracetamol tablets for the cold,achieving the molecule structural information of tablets without any pre treatment.In the quantitative analysis of tablets by DESI-MS,the tablets of standard paracetamol were made starch used as the main matrix to avoid the effect of matrix on ionizations.Under the optimized conditions,this method was applied in the quantitative detection of paracetamol in real tablets.Results showed that there was a good linear relationship for paracetamol in the range of 035-452 mg/mm2 with a correlation coefficient(r2) of 0998 2.The limit of quantitation and limit of detection were 1903 ng/mm2 and 0237 ng/mm2,respectively.The spiked recoveries for paracetamol were in the range of 102%-114%.The method was used for the direct detection of paracetamol in three commercial paracetamol tablets.Compared with the data provided by the pharmaceutical manufacturers,the relative standard deviations(RSD) of 72%-12% were obtained.The present work confirmed that,with the advantages of drugs rapid detection,DESI-MS provided an efficient and effective tool for quality control of drugs.关键词：desorption electrospray ionization mass spectrometry(DESI-MS);cold tablets;paracetamol;rapid detection of drugs
- 1882
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- 5
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- 1
发布时间：2023-05-25 - 摘要：A liquid chromatography-mass spectrometry with microdialysis was used to screen potential α glucosidase inhibitors in the extracts of Scutellaria baicalensis and identify the structures of those bioactive components screened.The chromatographic separation was carried out on a Dikma C18 column(150 mm×46 mm,5 μm) by gradient elution with 05% acetic acid solution-acetonitrile as mobile phases at a flow rate of 05 mL/min and a column temperature of 30 ℃.Mass spectrometry analysis and data acquisition were conducted in the positive ion mode.In this work,ten potential α glucosidase inhibitors in Scutellaria baicalensis were found and identified simultaneously.The binding degrees of 10 compounds with α glucosidase ranged from 3618% to 5271%.With the advantages of rapidness,high throughput and effectiveness,this method could screen α glucosidase inhibitors in Scutellaria baicalensis and provide valuable information for screening α glucosidase inhibitors from other traditional Chinese medicines.关键词：Scutellaria baicalensis;α glucosidase;microdialysis;HPLC-MSn;inhibitor
- 1939
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- 5
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- 2
发布时间：2023-05-25 - 摘要：An online solid phase extraction-high performance liquid chromatographic(Online SPE-HPLC) method was developed for the determination of mycophenolic acid in human plasma.Plasma samples were directly injected into the online SPE-HPLC system after simple protein precipitation.Capcell PAK MF Ph-1 was employed as an online SPE column and Poroshell 120 EC-C18 was employed as an analysis column.Results showed that there was a good linear relationship for mycophenolic acid in the concentration range of 020-5000 μg/mL,with a correlation coefficient(r) of 0999 8.The limit of detection(LOD) and limit of quantitation(LOQ) were of 007 μg/mL and 020 μg/mL,respectively.The spiked recoveries for mycophenolic acid in human plasma at three spiked levels of 039,2500 and 5000 μg/mL ranged from 962% to 105%,with intra assay relative standard deviations(intra RSD) of 26%-31% and inter assay relative standard deriation(inter RSD) of 29%-33%.The method was rapid and simple,and was suitable for the determination of mycophenolic acid concentrations in human plasma.关键词：mycophenolic acid;human plasma;online solid phase extraction-high performance liquid chromatography(online SPE-HPLC)
- 1857
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- 4
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发布时间：2023-05-25
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