An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in mic...An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in microalgae samples using ultra-high-performance liquid chromatographyquadrupole/Orbitrap high-resolution mass spectrometry(UPLC-Q/Orbitrap HRMS).The novel synthetic food was extracted using 50%methanol solution and purified with 3 mL of n-hexane saturated with 50%(volume fraction)methanol solution.For the microalgae samples,extraction was performed with 80%(volume fraction)acetonitrile solution and purified using a PRiME HLB solid-phase extraction column.An ACQUITY HSS T3 column(100 mm×2.1 mm,1.8μm)was used for analyte separation,with 5 mmol/L ammonium acetate containing 0.01%(volume fraction)formic acid and methanol selected as the mobile phase.Gradient elution was adopted.Data acquisition was conducted in both positive and negative modes in full-scan data-dependent secondary scan mode(full MS-ddMS2).Matrix-matched standards were employed for quantification in the external standard method.Additionally,mzVault and TraceFinder were used to establish a screening database for 28 food safety risk factors.The results showed that the relative deviation of the exact mass of 28 food safety risk factors was less than 5×10^(-6),with good linearity in the range of 1-100μg/kg,and a correlation coefficient(r^(2))of≥0.9978.The detection limit ranged from 0.5 to 4μg/kg,and the quantification limit ranged from 1 to 10μg/kg.The method recovery ranged from 70.0%to 119.6%with relative standard deviations ranging from 0.4%to 14.6%(n=6).The method is simple,sensitive,accurate,and suitable for rapid screening of 28 food safety risk factors in novel foods.展开更多
The widespread use of pesticides induces heavy adverse effects on human health,especially for the pregnant women and the newborns.In this study,a screening method has been developed for the determination of multi-pest...The widespread use of pesticides induces heavy adverse effects on human health,especially for the pregnant women and the newborns.In this study,a screening method has been developed for the determination of multi-pesticides in maternal and umbilical cord sera.All pesticides in sera were collected using solid phase extraction(SPE),and analyzed by gas chromatography-quadrupole time of flight mass spectrometry(GC-QTOF MS).To set up the quality criteria,a database of 50 pesticides was created and the accurate masses of 3 up to 5 representative ions with their intensity ratios were included for each pesticide.In addition,a novel"identification points"(IPs)system relying on the accurate MS1 and MS2 spectra was used to interpret the data for each suspected pesticide.The methodology was then applied to a pair of maternal and umbilical cord sera.A total of six pesticide residues were screened out successfully.In conclusion,GC-QTOF MS combined with an accurate mass database seemed to be one of the most efficient tools for systematic pesticide analysis.展开更多
Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives:...Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives: The purpose of this study is to clarify the bioactive mechanism of CWR in treating blood stasis. Materials and Methods: In this study, pharmacological indexes, including hemorheology and four blood coagulation indexes were tested. Bile and urine metabolomics were engaged by UPLC-Q/TOF-MS. Multivariate statistical analysis were used to screen out differential endogenous metabolites. Results: The results indicated that CWR significantly ameliorated the hemorheology and coagulation functions of acute blood stasis(ABS) model rats. Moreover, 27 endogenous metabolites between the CWR group and the ABS group were screened, and the levels were all improved to certain degrees by CWR preadministration. Metabonomics results indicated that ABS was mainly related to linoleic acid metabolism, arachidonic acid metabolism, glycerophospholipid metabolism, sphingolipid metabolism, pentose and glucuronate intercereasonversions, steroid hormone biosynthesis, and primary bile acid biosynthesis. Conclusion: In a word, the metabolomics method is consistent with the holistic view of traditional Chinese medicine(TCM) that can be a powerful means to illustrate the biological activity mechanism of CWR in treating blood stasis and to offer research demonstration for further study on the effector mechanism of TCM.展开更多
The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of ris...The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of risk substances(including local anesthetics,LAs)in cosmetics,which has been successfully applied in the analysis of actual samples.This work aims to develop a more convenient high performance liquid chromatography triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method for the quantitative determination of LAs.Samples were ultrasonically extracted with methanol,separated on an Agilent Poroshell 120 EC-C18 column(2.1 mm×100 mm,2.7μm),and eluted with a gradient mobile phase consisting of 0.1%formic acid aqueous solution and methanol.Quantification was performed using the external standard method.The results show that all 23 LAs are effectively separated within 12 minutes,with good linearity in the corresponding concentration ranges and the correlation coefficients all greater than 0.99.The limits of detection(LOD)range from 0.0025 to 0.05μg/g,and the limits of quantification(LOQ)range from 0.01 to 0.1μg/g.The average recoveries of the 23 LAs in 5 blank cosmetic matrices are 80.68%-117.57%,with the relative standard deviations(RSDs)less than 5.98%.This method has good precision and high accuracy,and is suitable for the determination of LAs in 5 cosmetic matrices.展开更多
BACKGROUND Primary biliary cholangitis(PBC)and autoimmune hepatitis(AIH)are two unexplained immune diseases.The golden standard for diagnosis of these diseases requires a liver biopsy.Liver biopsy is not widely accept...BACKGROUND Primary biliary cholangitis(PBC)and autoimmune hepatitis(AIH)are two unexplained immune diseases.The golden standard for diagnosis of these diseases requires a liver biopsy.Liver biopsy is not widely accepted by patients because of its invasive nature,and atypical liver histology can confuse diagnosis.In view of the lack of effective diagnostic markers for PBC and AIH,combined with the increasingly mature metabolomics technologies,including full-contour metabolomics and target.AIM To determine non-invasive,reliable,and sensitive biochemical markers for the differential diagnosis of PBC and AIH.METHODS Serum samples from 54 patients with PBC,26 patients with AIH and 30 healthy controls were analyzed by Ultra-high performance liquid chromatographytandem mass spectrometry serum metabolomics.The metabolites and metabolic pathways were identified,and the metabolic changes,metabolic pathways and inter-group differences between PBC and AIH were analyzed.Fifteen kinds of target metabolites of bile acids(BAs)were quantitatively analyzed by SRM,and the differential metabolites related to the diagnosis of PBC were screened by receiver operating characteristic curve analysis.RESULTS We found the changes in the levels of amino acids,BAs,organic acids,phospholipids,choline,sugar,and sugar alcohols in patients with PBC and AIH.Furthermore,the SRM assay of BAs revealed the increased levels of chenodeoxycholic acid,lithocholic acid(LCA),taurolithocholic acid(TLCA),and LCA+TLCA in the PBC group compared with those in the AIH group.The levels of BAs may be used as biomarkers to differentiate PBC from AIH diseases.The levels of glycochenodeoxycholic acid,glycochenodeoxycholic sulfate,and taurodeoxycholic acid were gradually elevated with the increase of Child-Pugh class,which was correlated with the severity of disease.CONCLUSION The results demonstrated that the levels of BAs could serve as potential biomarkers for the early diagnosis and assessment of the severity of PBC and AIH.展开更多
OBJECTIVE:To analyze the serum metabolic targets of the"Zhibian(BL54)through Shuidao(ST28)"acupuncture technique in cyclophosphamide(CTX)-induced premature ovarian insufficiency(POI)model rats and to elucida...OBJECTIVE:To analyze the serum metabolic targets of the"Zhibian(BL54)through Shuidao(ST28)"acupuncture technique in cyclophosphamide(CTX)-induced premature ovarian insufficiency(POI)model rats and to elucidate the potential molecular mechanism of acupuncture in improving POI.METHODS:We used an intraperitoneal injection of CTX to establish the POI rat model(POI group)and compared serum hormone levels and ovarian histopathological changes to evaluate the effect of the Zhibian(BL54)through Shuidao(ST28)technique(ZS+POI group)on ovarian function.Then,nontargeted metabolomics was performed using rat serum by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF/MS).RESULTS:After acupuncture intervention,the serum hormone levels and ovarian pathological morphology of POI rats were effectively improved.Moreover,UPLC-Q-TOF/MS results showed that the ZS+POI group showed a significant reversal of the levels of 6 differential metabolites.Among them,the levels of four serum metabolic markers,divanillyltetrahydrofuran ferulate,trans-ferulic acid,tryptamine,and neuraminic acid,increased significantly.Further analysis of biological effects showed that all metabolites were involved in the regulation of reproductive hormone levels and antioxidant and antiapoptotic effects.CONCLUSIONS:The"Zhibian(BL54)through Shuidao(ST28)"acupuncture method may improve the ovarian function of POI rats by regulating serum metabolite markers to exert antioxidant and antiapoptotic effects,which provides a theoretical basis for the clinical application of acupuncture in the treatment of POI.展开更多
Objective: To bioprospect optimal phenological phases as source of novel molecules from native golden yellow Pleurotus citrinopileatus across four phenologies in both aqueous and ethanol extracts, and identify novel m...Objective: To bioprospect optimal phenological phases as source of novel molecules from native golden yellow Pleurotus citrinopileatus across four phenologies in both aqueous and ethanol extracts, and identify novel molecules responsible for these activities.Methods: Standard qualitative assay, Folin–Ciocalteu assay; aluminium chloride spectrophotometric, 2, 2-diphenyl-1-picrylhydrazyl, 2, 20-azinobis(3-ethylbenzothiazoline-6-suslfonic acid, ferricyanide reducing antioxidant power were used to determine total flavonoid, polyphenols, radical scavenging, and reducing power. Spectrophotometric methods were used for lycopene, b-carotene, and total carotenoids, while liquid chromatography quadrupole time of flight mass spectrometry was used for identification and comparative quantitation of polyphenols and flavonoids across the four phenological states. Chem Spider? database was used for the identification of compounds based on their empirical formula, accurate mass and literature review of previously reported compounds in mushroom.Results: Primordial phases exhibited higher contents of secondary metabolites than mature basidiocarps. Polyphenols content differed across physiological phases with primordials exhibiting significant high contents(P < 0.05) [(13.803 ± 0.797) mg gallic acid equivalent/g dry weight]. Distribution of total flavonoids was significantly different(P < 0.05) across physiological states and ranged from(3.311 ± 0.730) to(14.824 ± 0.890) mg quercetin equivalent g dry weight. Ten polyphenol acids and seven flavonoids compounds identified varied across these phases with primordials exhibiting relatively high peak areas. Total antioxidant activities showed a positive correlation with total polyphenols(r = 0.969;P < 0.05) and total flavonoids(r = 0.960; P < 0.05) across these phenologies.Conclusions: These findings provide evidence that primordials of golden yellow mushroom as opposed to their fruiting bodies are potent sources of bioactive health molecules.展开更多
Objective:Cholesteryl esters(CEs)are composed of various fatty acyl chains attached to the hydroxyl groups of cholesterol,and abnormalities in their metabolism are related to many diseases.This study aimed to develop ...Objective:Cholesteryl esters(CEs)are composed of various fatty acyl chains attached to the hydroxyl groups of cholesterol,and abnormalities in their metabolism are related to many diseases.This study aimed to develop an ultrahigh-performance liquid chromatography-quadrupole exactive mass spectrometry(UPLC-Q-Exactive MS)method to identify the CEs in plasma.Methods:First,the MS fragmentation patterns were investigated using seven commercial CE standards.Then,the CEs in plasma were characterized through the accurate mass data of precursor ions and characteristic product ions.A strategy of step-by-step m/z scans in a narrow range was proposed to identify more trace CEs by the full-scan data-dependent MS/MS(ddMS2)mode.Results:A total of 50 CE species consisting of 55 regioisomers were identified in human plasma.Among them,two species were reported for the first time.Conclusion:This study is the most comprehensive identification of CE species in human plasma to date.These results will contribute to the in-depth profiling of CEs in human plasma and provide guidance for animal model selection when studying lipid-related diseases.展开更多
[Objectives]To use liquid chromatography-mass spectrometry technology to analyze the chemical composition of traditional Chinese medicine and explore its application in the evaluation of quality stability of tradition...[Objectives]To use liquid chromatography-mass spectrometry technology to analyze the chemical composition of traditional Chinese medicine and explore its application in the evaluation of quality stability of traditional Chinese medicine.[Methods]Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS)was used to detect the samples of Moluodan concentrated pills.By comparing and analyzing the detection results of 10 different batches of Moluodan concentrated pills,combined with principal component analysis(PCA),the quality stability of Moluodan concentrated pills was evaluated.[Results]A total of 367 chemical components were identified in Moluodan concentrated pills.The average repetition rate of the chemical components contained in the 10 different batches of samples reached 92%.The overall quality stability of the Moluodan concentrated pills was good.[Conclusions]The UPLC-QTOF-MS technology combined with PCA provides a reference for the overall quality evaluation of Moluodan concentrated pills,and provides new detection methods and ideas for the analysis of the components of Chinese medicine.展开更多
Background:Rising insulin poisoning cases demand more reliable forensic biomarkers as current diagnostic methods face accuracy limitations,highlighting metabolomics’potential for identifying acute intoxication marker...Background:Rising insulin poisoning cases demand more reliable forensic biomarkers as current diagnostic methods face accuracy limitations,highlighting metabolomics’potential for identifying acute intoxication markers.Aims and Objectives:This study aimed to investigate changes in serum metabolites in rats with acute insulin poisoning using untargeted metabolomics and to identify endogenous metabolic signatures highly associated with acute insulin poisoning,thereby providing auxiliary evidence for forensic identification of insulin intoxication.Materials and Methods:Rat models were established for the control group,low-dose insulin group,and high-dose insulin group.Ultra-high-performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry(UPLC-Q-Exactive Orbitrap MS)was employed to profile endogenous serum metabolites.Bioinformatics methods were applied to screen characteristic metabolites related to acute insulin poisoning based on variable importance in projection values from the orthogonal partial least squares-discriminant analysis model and fold change values.Pathway analysis was then performed on the identified metabolites.Results:A total of 18 differential metabolites unrelated to insulin dosage were screened,among which four metabolites were upregulated and 14 were downregulated in the insulin-treated groups.These small-molecule metabolites were primarily enriched in the sphingolipid metabolism and primary bile acid biosynthesis pathways.Conclusions:Insulin poisoning induces alterations in small-molecule metabolites in vivo.The identified differential metabolites may serve as auxiliary indicators for forensic determination of insulin intoxication.展开更多
Objective To clarify the potential mechanism of Banxia Xiexin Decoction(BXD)on colorectal cancer(CRC)from the perspective of metabolomics.Methods Forty male C57BL/6 mice were randomly divided into normal control(NC),a...Objective To clarify the potential mechanism of Banxia Xiexin Decoction(BXD)on colorectal cancer(CRC)from the perspective of metabolomics.Methods Forty male C57BL/6 mice were randomly divided into normal control(NC),azoxymethane/dextran sulfate sodium(AOM/DSS)model,low-dose BXD(L-BXD),high-dose BXD(H-BXD)and mesalamine(MS)groups according to a random number table,8 mice in each group.Colorectal cancer model was induced by AOM/DSS.BXD was administered daily at doses of 3.915(L-BXD)and 15.66 g/kg(H-BXD)by gavage for consecutive 21 days,and 100 mg/kg MS was used as positive control.Following the entire modeling cycle,colon length of mice was measured and quantity of colorectal tumors were counted.The spleen and thymus index were determined by calculating the spleen/thymus weight to body weight.Inflammatory cytokine and changes of serum metabolites were analyzed by enzyme-linked immunosorbent assay kits and ultra performance liquid chromatography-quadrupole/time-of-flight mass spectrometry(UPLC-Q/TOF-MS),respectively.Results Notably,BXD supplementation protected against weight loss,mitigated tumor formation,and diminished histologic damage in mice treated with AOM/DSS(P<0.05 or P<0.01).Moreover,BXD suppressed expression of serum inflammatory enzymes,and improved the spleen and thymus index(P<0.05).Compared with the normal group,102 kinds of differential metabolites were screened in the AOM/DSS group,including 48 potential biomarkers,involving 18 main metabolic pathways.Totally 18 potential biomarkers related to CRC were identified,and the anti-CRC mechanism of BXD was closely related to D-glutamine and D-glutamate metabolism,phenylalanine,tyrosine and tryptophan biosynthesis,arginine biosynthesis,nitrogen metabolism and so on.Conclusion BXD exerts partial protective effects on AOM/DSS-induced CRC by reducing inflammation,protecting organism immunity ability,and regulating amino acid metabolism.展开更多
To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolutio...To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.展开更多
To effectively utilize apple pomace resources,we extracted apple pomace polyphenols using natural deep eutectic solvent(NADES)as the medium,with a solvent-to-solid ratio of 50 mL/g,for a duration of 120 min.Compared t...To effectively utilize apple pomace resources,we extracted apple pomace polyphenols using natural deep eutectic solvent(NADES)as the medium,with a solvent-to-solid ratio of 50 mL/g,for a duration of 120 min.Compared to conventional extraction solvents(ethanol and methanol),four NADES significantly enhanced the extraction efficiency of polyphenols from apple pomace.Notably,NADES 1(betaine:urea=1:1,30% water)and NADES 2(betaine:malic acid=1:1,30% water)exhibited superior extraction capabilities,with maximum values reaching 5.245±0.124 mg GAE/g pomace and 5.157±0.164 mg GAE/g pomace,respectively,in Qinguan apple pomace.Both solvents reached their maximum extraction efficiency within 120 min,with NADES 1 achieving a maximum extraction amount of 4.8325 mg GAE/g and NADES 2 achieving 5.3039 mg GAE/g from Fuji apple pomace.NADES 1 and NADES 2 were more efficient in extracting monophenols such as quercetin,rutin,gallic acid,and procyanidin,whereas organic solvents(methanol and ethanol)were more effective for monophenols like methyl gallate and phlorizin.Furthermore,polyphenol extracts obtained using NADES from Fuji apple pomace displayed varying levels of antibacterial effectiveness,with NADES 4(glucose:lactic acid=1:5,60% water)and NADES 2 showing superior efficacy against Escherichia coli and Staphylococcus aureus.This comprehensive study not only demonstrated the potential of NADES in extracting polyphenols from apple pomace but also highlighted their applicability as natural preservatives in the food industry.展开更多
基金supported by the National Key Research and Development Program for Young Scientists of China(No.2022YFF1102900).
文摘An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in microalgae samples using ultra-high-performance liquid chromatographyquadrupole/Orbitrap high-resolution mass spectrometry(UPLC-Q/Orbitrap HRMS).The novel synthetic food was extracted using 50%methanol solution and purified with 3 mL of n-hexane saturated with 50%(volume fraction)methanol solution.For the microalgae samples,extraction was performed with 80%(volume fraction)acetonitrile solution and purified using a PRiME HLB solid-phase extraction column.An ACQUITY HSS T3 column(100 mm×2.1 mm,1.8μm)was used for analyte separation,with 5 mmol/L ammonium acetate containing 0.01%(volume fraction)formic acid and methanol selected as the mobile phase.Gradient elution was adopted.Data acquisition was conducted in both positive and negative modes in full-scan data-dependent secondary scan mode(full MS-ddMS2).Matrix-matched standards were employed for quantification in the external standard method.Additionally,mzVault and TraceFinder were used to establish a screening database for 28 food safety risk factors.The results showed that the relative deviation of the exact mass of 28 food safety risk factors was less than 5×10^(-6),with good linearity in the range of 1-100μg/kg,and a correlation coefficient(r^(2))of≥0.9978.The detection limit ranged from 0.5 to 4μg/kg,and the quantification limit ranged from 1 to 10μg/kg.The method recovery ranged from 70.0%to 119.6%with relative standard deviations ranging from 0.4%to 14.6%(n=6).The method is simple,sensitive,accurate,and suitable for rapid screening of 28 food safety risk factors in novel foods.
基金supported by the Science and Technology Commission of Shanghai Municipality(13ZR1448100)
文摘The widespread use of pesticides induces heavy adverse effects on human health,especially for the pregnant women and the newborns.In this study,a screening method has been developed for the determination of multi-pesticides in maternal and umbilical cord sera.All pesticides in sera were collected using solid phase extraction(SPE),and analyzed by gas chromatography-quadrupole time of flight mass spectrometry(GC-QTOF MS).To set up the quality criteria,a database of 50 pesticides was created and the accurate masses of 3 up to 5 representative ions with their intensity ratios were included for each pesticide.In addition,a novel"identification points"(IPs)system relying on the accurate MS1 and MS2 spectra was used to interpret the data for each suspected pesticide.The methodology was then applied to a pair of maternal and umbilical cord sera.A total of six pesticide residues were screened out successfully.In conclusion,GC-QTOF MS combined with an accurate mass database seemed to be one of the most efficient tools for systematic pesticide analysis.
基金financially supported by the National Natural Science Foundation of China (81673598, 81973483, 82003948)Natural Science Foundation of Zhejiang Province (LQ21H280002)+3 种基金The National Key Research and Development Program of China (2018YFC1707000)the National traditional Chinese medicine industry special project (2015468002-2)National Standardization Program for Chinese Medicine (ZYBZH-Y-SC-40)Zhejiang Chinese Medicine University School-level Scientific Research Fund for Talents (2020ZR14)。
文摘Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives: The purpose of this study is to clarify the bioactive mechanism of CWR in treating blood stasis. Materials and Methods: In this study, pharmacological indexes, including hemorheology and four blood coagulation indexes were tested. Bile and urine metabolomics were engaged by UPLC-Q/TOF-MS. Multivariate statistical analysis were used to screen out differential endogenous metabolites. Results: The results indicated that CWR significantly ameliorated the hemorheology and coagulation functions of acute blood stasis(ABS) model rats. Moreover, 27 endogenous metabolites between the CWR group and the ABS group were screened, and the levels were all improved to certain degrees by CWR preadministration. Metabonomics results indicated that ABS was mainly related to linoleic acid metabolism, arachidonic acid metabolism, glycerophospholipid metabolism, sphingolipid metabolism, pentose and glucuronate intercereasonversions, steroid hormone biosynthesis, and primary bile acid biosynthesis. Conclusion: In a word, the metabolomics method is consistent with the holistic view of traditional Chinese medicine(TCM) that can be a powerful means to illustrate the biological activity mechanism of CWR in treating blood stasis and to offer research demonstration for further study on the effector mechanism of TCM.
文摘The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)qualitative method for screening more than 2000 kinds of risk substances(including local anesthetics,LAs)in cosmetics,which has been successfully applied in the analysis of actual samples.This work aims to develop a more convenient high performance liquid chromatography triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method for the quantitative determination of LAs.Samples were ultrasonically extracted with methanol,separated on an Agilent Poroshell 120 EC-C18 column(2.1 mm×100 mm,2.7μm),and eluted with a gradient mobile phase consisting of 0.1%formic acid aqueous solution and methanol.Quantification was performed using the external standard method.The results show that all 23 LAs are effectively separated within 12 minutes,with good linearity in the corresponding concentration ranges and the correlation coefficients all greater than 0.99.The limits of detection(LOD)range from 0.0025 to 0.05μg/g,and the limits of quantification(LOQ)range from 0.01 to 0.1μg/g.The average recoveries of the 23 LAs in 5 blank cosmetic matrices are 80.68%-117.57%,with the relative standard deviations(RSDs)less than 5.98%.This method has good precision and high accuracy,and is suitable for the determination of LAs in 5 cosmetic matrices.
基金Supported by Health and Family Planning Commission Project of Jilin Province,No.2016Q043Health and Hygiene Committee Project of Jilin Province,No.2021LC082。
文摘BACKGROUND Primary biliary cholangitis(PBC)and autoimmune hepatitis(AIH)are two unexplained immune diseases.The golden standard for diagnosis of these diseases requires a liver biopsy.Liver biopsy is not widely accepted by patients because of its invasive nature,and atypical liver histology can confuse diagnosis.In view of the lack of effective diagnostic markers for PBC and AIH,combined with the increasingly mature metabolomics technologies,including full-contour metabolomics and target.AIM To determine non-invasive,reliable,and sensitive biochemical markers for the differential diagnosis of PBC and AIH.METHODS Serum samples from 54 patients with PBC,26 patients with AIH and 30 healthy controls were analyzed by Ultra-high performance liquid chromatographytandem mass spectrometry serum metabolomics.The metabolites and metabolic pathways were identified,and the metabolic changes,metabolic pathways and inter-group differences between PBC and AIH were analyzed.Fifteen kinds of target metabolites of bile acids(BAs)were quantitatively analyzed by SRM,and the differential metabolites related to the diagnosis of PBC were screened by receiver operating characteristic curve analysis.RESULTS We found the changes in the levels of amino acids,BAs,organic acids,phospholipids,choline,sugar,and sugar alcohols in patients with PBC and AIH.Furthermore,the SRM assay of BAs revealed the increased levels of chenodeoxycholic acid,lithocholic acid(LCA),taurolithocholic acid(TLCA),and LCA+TLCA in the PBC group compared with those in the AIH group.The levels of BAs may be used as biomarkers to differentiate PBC from AIH diseases.The levels of glycochenodeoxycholic acid,glycochenodeoxycholic sulfate,and taurodeoxycholic acid were gradually elevated with the increase of Child-Pugh class,which was correlated with the severity of disease.CONCLUSION The results demonstrated that the levels of BAs could serve as potential biomarkers for the early diagnosis and assessment of the severity of PBC and AIH.
基金the Research Grant from the Natural Science Research Program of Shanxi Province:Based on Ultra-Performance Liquid Chromatography-Mass Spectrometry,the effect of"Zhibian(BL54)through Shuidao(ST28)"Needle Method on Ovarian Metabolism and Apoptosis Pathways in rats with Premature Ovarian Insufficiency was Discussed(No.2022030211216)。
文摘OBJECTIVE:To analyze the serum metabolic targets of the"Zhibian(BL54)through Shuidao(ST28)"acupuncture technique in cyclophosphamide(CTX)-induced premature ovarian insufficiency(POI)model rats and to elucidate the potential molecular mechanism of acupuncture in improving POI.METHODS:We used an intraperitoneal injection of CTX to establish the POI rat model(POI group)and compared serum hormone levels and ovarian histopathological changes to evaluate the effect of the Zhibian(BL54)through Shuidao(ST28)technique(ZS+POI group)on ovarian function.Then,nontargeted metabolomics was performed using rat serum by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF/MS).RESULTS:After acupuncture intervention,the serum hormone levels and ovarian pathological morphology of POI rats were effectively improved.Moreover,UPLC-Q-TOF/MS results showed that the ZS+POI group showed a significant reversal of the levels of 6 differential metabolites.Among them,the levels of four serum metabolic markers,divanillyltetrahydrofuran ferulate,trans-ferulic acid,tryptamine,and neuraminic acid,increased significantly.Further analysis of biological effects showed that all metabolites were involved in the regulation of reproductive hormone levels and antioxidant and antiapoptotic effects.CONCLUSIONS:The"Zhibian(BL54)through Shuidao(ST28)"acupuncture method may improve the ovarian function of POI rats by regulating serum metabolite markers to exert antioxidant and antiapoptotic effects,which provides a theoretical basis for the clinical application of acupuncture in the treatment of POI.
基金Supported by the African Union(African UnionNo.17/2014)
文摘Objective: To bioprospect optimal phenological phases as source of novel molecules from native golden yellow Pleurotus citrinopileatus across four phenologies in both aqueous and ethanol extracts, and identify novel molecules responsible for these activities.Methods: Standard qualitative assay, Folin–Ciocalteu assay; aluminium chloride spectrophotometric, 2, 2-diphenyl-1-picrylhydrazyl, 2, 20-azinobis(3-ethylbenzothiazoline-6-suslfonic acid, ferricyanide reducing antioxidant power were used to determine total flavonoid, polyphenols, radical scavenging, and reducing power. Spectrophotometric methods were used for lycopene, b-carotene, and total carotenoids, while liquid chromatography quadrupole time of flight mass spectrometry was used for identification and comparative quantitation of polyphenols and flavonoids across the four phenological states. Chem Spider? database was used for the identification of compounds based on their empirical formula, accurate mass and literature review of previously reported compounds in mushroom.Results: Primordial phases exhibited higher contents of secondary metabolites than mature basidiocarps. Polyphenols content differed across physiological phases with primordials exhibiting significant high contents(P < 0.05) [(13.803 ± 0.797) mg gallic acid equivalent/g dry weight]. Distribution of total flavonoids was significantly different(P < 0.05) across physiological states and ranged from(3.311 ± 0.730) to(14.824 ± 0.890) mg quercetin equivalent g dry weight. Ten polyphenol acids and seven flavonoids compounds identified varied across these phases with primordials exhibiting relatively high peak areas. Total antioxidant activities showed a positive correlation with total polyphenols(r = 0.969;P < 0.05) and total flavonoids(r = 0.960; P < 0.05) across these phenologies.Conclusions: These findings provide evidence that primordials of golden yellow mushroom as opposed to their fruiting bodies are potent sources of bioactive health molecules.
基金supported by National Natural Science Foundation of China(No.81874309,No.81903901 and No.81803717)the Youth Foundation of the Zhejiang Academy of Medical Sciences(No.2020Y003).
文摘Objective:Cholesteryl esters(CEs)are composed of various fatty acyl chains attached to the hydroxyl groups of cholesterol,and abnormalities in their metabolism are related to many diseases.This study aimed to develop an ultrahigh-performance liquid chromatography-quadrupole exactive mass spectrometry(UPLC-Q-Exactive MS)method to identify the CEs in plasma.Methods:First,the MS fragmentation patterns were investigated using seven commercial CE standards.Then,the CEs in plasma were characterized through the accurate mass data of precursor ions and characteristic product ions.A strategy of step-by-step m/z scans in a narrow range was proposed to identify more trace CEs by the full-scan data-dependent MS/MS(ddMS2)mode.Results:A total of 50 CE species consisting of 55 regioisomers were identified in human plasma.Among them,two species were reported for the first time.Conclusion:This study is the most comprehensive identification of CE species in human plasma to date.These results will contribute to the in-depth profiling of CEs in human plasma and provide guidance for animal model selection when studying lipid-related diseases.
基金Youth Project of Natural Science Foundation of Hebei Province(C2019402141)Science and Technology Research Project for Colleges and Universities in Hebei Province(QN2019215)Science and Technology Research and Development Plan of Handan City(1727201061).
文摘[Objectives]To use liquid chromatography-mass spectrometry technology to analyze the chemical composition of traditional Chinese medicine and explore its application in the evaluation of quality stability of traditional Chinese medicine.[Methods]Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS)was used to detect the samples of Moluodan concentrated pills.By comparing and analyzing the detection results of 10 different batches of Moluodan concentrated pills,combined with principal component analysis(PCA),the quality stability of Moluodan concentrated pills was evaluated.[Results]A total of 367 chemical components were identified in Moluodan concentrated pills.The average repetition rate of the chemical components contained in the 10 different batches of samples reached 92%.The overall quality stability of the Moluodan concentrated pills was good.[Conclusions]The UPLC-QTOF-MS technology combined with PCA provides a reference for the overall quality evaluation of Moluodan concentrated pills,and provides new detection methods and ideas for the analysis of the components of Chinese medicine.
基金support and sponsorship This research was supported by funding from the National Key Research and Development Program of China(2023YFC3303904)the Key Program of National Natural Science Foundation of China(82130056).
文摘Background:Rising insulin poisoning cases demand more reliable forensic biomarkers as current diagnostic methods face accuracy limitations,highlighting metabolomics’potential for identifying acute intoxication markers.Aims and Objectives:This study aimed to investigate changes in serum metabolites in rats with acute insulin poisoning using untargeted metabolomics and to identify endogenous metabolic signatures highly associated with acute insulin poisoning,thereby providing auxiliary evidence for forensic identification of insulin intoxication.Materials and Methods:Rat models were established for the control group,low-dose insulin group,and high-dose insulin group.Ultra-high-performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry(UPLC-Q-Exactive Orbitrap MS)was employed to profile endogenous serum metabolites.Bioinformatics methods were applied to screen characteristic metabolites related to acute insulin poisoning based on variable importance in projection values from the orthogonal partial least squares-discriminant analysis model and fold change values.Pathway analysis was then performed on the identified metabolites.Results:A total of 18 differential metabolites unrelated to insulin dosage were screened,among which four metabolites were upregulated and 14 were downregulated in the insulin-treated groups.These small-molecule metabolites were primarily enriched in the sphingolipid metabolism and primary bile acid biosynthesis pathways.Conclusions:Insulin poisoning induces alterations in small-molecule metabolites in vivo.The identified differential metabolites may serve as auxiliary indicators for forensic determination of insulin intoxication.
基金Supported by the Natural Science Foundation of Nanjing University of Chinese Medicine(No.XZR2020038)Science and Technology Innovation Project of Suzhou Medical and Health Care(No.SKJY2021136)Fifth Batch of Gusu Health Personnel Training Project in Suzhou(No.GSWS2020085)。
文摘Objective To clarify the potential mechanism of Banxia Xiexin Decoction(BXD)on colorectal cancer(CRC)from the perspective of metabolomics.Methods Forty male C57BL/6 mice were randomly divided into normal control(NC),azoxymethane/dextran sulfate sodium(AOM/DSS)model,low-dose BXD(L-BXD),high-dose BXD(H-BXD)and mesalamine(MS)groups according to a random number table,8 mice in each group.Colorectal cancer model was induced by AOM/DSS.BXD was administered daily at doses of 3.915(L-BXD)and 15.66 g/kg(H-BXD)by gavage for consecutive 21 days,and 100 mg/kg MS was used as positive control.Following the entire modeling cycle,colon length of mice was measured and quantity of colorectal tumors were counted.The spleen and thymus index were determined by calculating the spleen/thymus weight to body weight.Inflammatory cytokine and changes of serum metabolites were analyzed by enzyme-linked immunosorbent assay kits and ultra performance liquid chromatography-quadrupole/time-of-flight mass spectrometry(UPLC-Q/TOF-MS),respectively.Results Notably,BXD supplementation protected against weight loss,mitigated tumor formation,and diminished histologic damage in mice treated with AOM/DSS(P<0.05 or P<0.01).Moreover,BXD suppressed expression of serum inflammatory enzymes,and improved the spleen and thymus index(P<0.05).Compared with the normal group,102 kinds of differential metabolites were screened in the AOM/DSS group,including 48 potential biomarkers,involving 18 main metabolic pathways.Totally 18 potential biomarkers related to CRC were identified,and the anti-CRC mechanism of BXD was closely related to D-glutamine and D-glutamate metabolism,phenylalanine,tyrosine and tryptophan biosynthesis,arginine biosynthesis,nitrogen metabolism and so on.Conclusion BXD exerts partial protective effects on AOM/DSS-induced CRC by reducing inflammation,protecting organism immunity ability,and regulating amino acid metabolism.
基金supported by Science and Technology Program of the State Administration for Market Regulation of China (2020MK014).
文摘To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.
基金supported by grants from The National Key R&D Program of China(2023YFF130510403).
文摘To effectively utilize apple pomace resources,we extracted apple pomace polyphenols using natural deep eutectic solvent(NADES)as the medium,with a solvent-to-solid ratio of 50 mL/g,for a duration of 120 min.Compared to conventional extraction solvents(ethanol and methanol),four NADES significantly enhanced the extraction efficiency of polyphenols from apple pomace.Notably,NADES 1(betaine:urea=1:1,30% water)and NADES 2(betaine:malic acid=1:1,30% water)exhibited superior extraction capabilities,with maximum values reaching 5.245±0.124 mg GAE/g pomace and 5.157±0.164 mg GAE/g pomace,respectively,in Qinguan apple pomace.Both solvents reached their maximum extraction efficiency within 120 min,with NADES 1 achieving a maximum extraction amount of 4.8325 mg GAE/g and NADES 2 achieving 5.3039 mg GAE/g from Fuji apple pomace.NADES 1 and NADES 2 were more efficient in extracting monophenols such as quercetin,rutin,gallic acid,and procyanidin,whereas organic solvents(methanol and ethanol)were more effective for monophenols like methyl gallate and phlorizin.Furthermore,polyphenol extracts obtained using NADES from Fuji apple pomace displayed varying levels of antibacterial effectiveness,with NADES 4(glucose:lactic acid=1:5,60% water)and NADES 2 showing superior efficacy against Escherichia coli and Staphylococcus aureus.This comprehensive study not only demonstrated the potential of NADES in extracting polyphenols from apple pomace but also highlighted their applicability as natural preservatives in the food industry.
