An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracte...An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.展开更多
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s...A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.展开更多
Objectives: To study the characteristics of serum metabonomics in coronary heart disease (CHD) patients diagnosed as phlegm or blood stasis pattern and explore effects of formula-pattern correspondence treatment. M...Objectives: To study the characteristics of serum metabonomics in coronary heart disease (CHD) patients diagnosed as phlegm or blood stasis pattern and explore effects of formula-pattern correspondence treatment. Methods: A total of 102 stable CHD patients were enrolled and divided into phlegm group (P group, n=52) and blood stasis group (BS group, n=50) according to pattern identification. Gualou Xiebai Banxia Decoction (瓜萎薤白半夏汤, GXBD) and Xuefu Zhuyu Decoction (血府逐瘀汤, XZD) were used as drug interventions. Relevant indicators of metabonomics were observed by ultra performance liquid chromatography mass spectrometry (UPLC-MS) and pattern recognition. Results: Levels of amino acids and phosphatidylethanolamine (PE) in the CHD group were much higher than those in healthy control group, while the levels of unsaturated fatty acids, sphingosine, Lyso, phosphatidylcholine (PC) were significantly lower (P〈0.01). Most of the differential metabolites between the CHD and the healthy groups were also common metabolites of phlegm and blood stasis. 7(Z), 10(Z)- hexadecadienoic acid and DPA were decreased in the P group and increased in the BS group. According to the quantity of retraced metabolites, improvement in metabonomics by formula-pattern correspondence was superior to that without correspondence in the BS group. Based on the varieties of metabolites, GXBD could improve the levels of docosapentaenoic acid (DPA), sphingomyelin (SM) (d34:1), and L-Lactic acid and XZD could ameliorate the levels of sphingosine and Vit E in the P group, in the BS group, GXBD could improve vitamin E level and XZD could make improvements in the levels of octadecanoic acid, phosphoglycerol, and SM (d34:1). Conclusions: Phlegm and blood stasis in CHD patients present specific differential metabolites, and share common metabolites. Remarkable differences have been displayed in pathological properties and severity of phlegm and blood stasis. Patients with phlegm are more likely to have lipid metabolism disorders. However, in patients with blood stasis, problems mainly lie in glucose, protein and fat metabolism and the injury of vascular cell membrane is relatively severe. The metabolic disorder is more complicated in blood stasis pattem than that in phlegm pattem. Compared with non-correspondence, improvement of differential metabolites is more comprehensive and targeted in formulapattern correspondence with a better effect.展开更多
A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS) method was developed for the analysis of tetracycline antibiotics, including tetracycline (TC), oxyte...A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS) method was developed for the analysis of tetracycline antibiotics, including tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and their 4-epimers (4-epiTCs) in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution (pH 4.0), then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2:15:83 (v/v/v). The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method (LODsoil) ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.展开更多
Objective: To detect absorbed bioactive compounds of the water extract whose pharmacodynamic effect was craniocerebral protection for quality control assessment. Methods: Anthraquinones in water extract of rhubarb ...Objective: To detect absorbed bioactive compounds of the water extract whose pharmacodynamic effect was craniocerebral protection for quality control assessment. Methods: Anthraquinones in water extract of rhubarb (WER), in cerebrospinal fluid (CSF) of patients with traumatic brain injury (TBI) and in ipsilateral cortex of TBI rats following oral WER were respectively explored by ultra performance liquid chromatography with photodiode array detector (UPLC-PDA) method developed in the present study. The effects of anthraquinones absorbed into injured cortex on superoxidase dismutase (SOD) activity in TBI rats were detected. The antioxidative anthraquinones absorbed into target organ were evaluated for quality control of WER. Results: Anthraquinones in WER were aloe-emodin, rhein, emodin, chrysophanol, and physcion. Only the last anthraquinone was found in CSF and in ipsilateral cortex under this chromatographic condition. Physcion increased SOD activity in TBI rats significantly. Conclusions: Physcion was the main active compound of rhubarb against craniocerebral injury via antioxidant pathway. According to our strategy, the exploration of physcion suggested the possibility of a novel quality control of WER in treating TBI injury.展开更多
The enantiomer residues of metalaxyl, napropamide, triticonazole and metconazole were detected in soil by Qu EChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The soil sample was e...The enantiomer residues of metalaxyl, napropamide, triticonazole and metconazole were detected in soil by Qu EChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The soil sample was extracted with acetonitrile containing 1% acetic acid and purified using Qu ECh ERS method. Quantitative analysis for the enantiomers of these four chiral pesticides was performed in MS in multi-response monitoring(MRM) mode by external standard method. All enantiomers showed good linearity in the range of 0.5 to 50 μg/L. The average recoveries of enantiomers in soil were 81.74% to 105.79% with relative standard deviations(RSDs) from 3.69% to 7.86%. The method quantitative limit(MQL) was 5.3-30.3 ng/kg. The method can be used for rapid screening and determination of chiral pesticides in soil.展开更多
A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in n...A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in negative mode. Plant samples were extracted and cleaned up through florisil column, resolved on a 100 mm C18 column with linear gradient elution and detected by mass spectrometry in multiple reaction monitoring (MRM) mode. The method provided good recoveries rang- ing from 68.2% to 94.6%, relative standard deviation (RSD) in the range of 3.2% - 9.1%, and limits of quantification (LOQ) defined as the signal-to-noise ratio of 10 of 0.3-2.1 ng/g. It allowed a fast separation and sensitive quantification of the isomers and homologues of seven OH-PBDE congeners 2′-OH-BDE-3, 3′-OH-BDE-7, 4′-OH-BDE-17, 3′-OH-BDE-28, 3-OH-BDE-47, 5-OH-BDE-47 and 6-OH-BDE-47. The method was successfully applied to identify and quantify the formation of hydroxylat- ed metabolites in alfalfa exposed to BDE-209. Five OH-PBDEs were detected in plant tissues, and more congeners were found in roots than in shoots. To our knowledge, this work represents the first attempt to validate UPLC-MS/MS method to quantify OH-PBDEs in plant samples without derivatization.展开更多
A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tande...A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.展开更多
Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism...Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after展开更多
[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an H...[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value.展开更多
The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ket...The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ketchup,and the upper layer was detected by the UPLC-MS/MS after refrigeration and centrifuge.The sample was separated on a Waters Acquity BHE C18 column,and detected by the MRM mode of the mass spectrum.The LOD was 2 ng/mL and the LOQ was 5 ng/mL all of the four substances.The average recoveries were between 67.42%-84.59% of the 100,200,300 μg/kg three spiked concentration levels and the RSD values were between 2.87%-9.57%.展开更多
An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed s...An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed simultaneously with an Waters Acquity BHE C18 column by gradient elution using 0.05% aqueous ammonia-acetonitrile as mobile phase and detected by the MRM mode of the mass spectrum.The recoveries of the SPE method were between 68.79%-95.65% (RSD<7.94%,n=4),and all the alkaloids showed good linearity (r>0.998) in a relatively wide concentration range.The LOD reached 0.0516,0.0640,0.0744 ng/mL of aconitine,hypaconitine and mesaconitine,respectively.The analysis time was within 3 min which could meet the high-throughput detection.The results indicated that contents of alkaloids in animal blood can be well detected;and this method can be used in quality control of aconitum drugs and pharmacokinetics study.展开更多
Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of...Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of parathyroid hormone (PTH) in presence of meta-cresol as a stabilizer in a pharmaceutical formulation.Chromatography was performed with mobile phase containing 0.1% Trifluoroacetic acid (TFA) in MilliQ water and 0.1% TFA in acetonitrile with gradient program and flow rate at 0.3 mL/min for HPLC and 0.4 mL/min for UPLC.Quantification was accomplished with internal reference standard (qualified against innovator product and National Institute for Biological Standards and Control (NIBSC) standard).The methods were validated for linearity (correlation coefficient 0.99),range,accuracy,precision and robustness.Robustness was confirmed by considering three factors;mobile phase composition,column temperature and flow rate/age of mobile phase.Intermediate precision was confirmed on different equipments,different columns and on different days.The relative standard deviation (RSD) (<2% for RP-HPLC and <1% for UPLC,n=30) indicated a good precision.Retention time was found about 17 min and 2 min by HPLC and UPLC methods,respectively.Both methods are simple,highly sensitive,precise and accurate and have the potential of being useful for routine quality control.展开更多
[Objectives]To establish a UPLC-UV method for the determination of polydatin in the serum of Wistar rats.[Methods]Acquity UPLC BEH shield RP18 column(1.7μm,2.1 mm×100 mm,Waters Corporation,USA)was used as the an...[Objectives]To establish a UPLC-UV method for the determination of polydatin in the serum of Wistar rats.[Methods]Acquity UPLC BEH shield RP18 column(1.7μm,2.1 mm×100 mm,Waters Corporation,USA)was used as the analytical column,acetonitrile-water(55∶45)was used as the mobile phase,the flow rate was 0.5 mL/min,and the column temperature was 30℃and the detection wavelength was 306 nm.[Results]The linear range of the established serum sample analysis method was 1.0-20.0μg/mL,and the correlation coefficient was r=0.9994;the intraday and interday RSD of Wistar rat serum was less than 3.0%,and the accuracy was higher than 90%.[Conclusions]This method is sensitive,accurate,and rapid.It is suitable for monitoring the concentration of polydatin in serum after intragastric administration,and can also be used for pharmacokinetics and bioavailability studies.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
Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A (BPA), nonylphenol (NP), and octylphenol (OP) in urine samples. Methods Sixty uri...Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A (BPA), nonylphenol (NP), and octylphenol (OP) in urine samples. Methods Sixty urine samples collected from healthy subjects were analyzed for BPA, NP, and OP concentrations. The samples were de‐conjugated by adding β‐glucuronidase and sulfatase. After the enzymatic treatment, the samples were subjected to the OASIS HLB column solid phase extraction cartridges so as to be cleaned and concentrated. The UPLC separation was performed on a Acquity UPLCTM BEH C18 column (2.1×100 mm, 1.7 μm) with a gradient elution system of methanol‐water as the mobile phase. Triple‐quadrupole mass spectrometry analyzer was used for the qualitative and quantitative analysis of UPLC‐MS/MS system. Results The limit of detection of BPA, NP, and OP was 0.10, 0.10, and 0.15 ng/mL, respectively. The recoveries of BPA, NP and OP were 80.1%‐108%, 81.3%‐109%, and 81.5%‐98.7%, respectively. Among the 60 urine samples, BPA was detected in 8 samples at the level of 0.297‐32.7ng/mL, NP was detected in 29 samples at the level of 1.69‐27.8 ng/mL, and OP was detected in 17 samples at the level of 0.407‐11.1 ng/mL. Conclusion The method is simple with high sensitivity and selectivity, and is suitable for the determination of BPA, NP, and OP in urine. As shown by our analysis , BPA, NP, and OP appear to be prevalent in human urine. This is particularly true for NP. The results from our study is therefore valuable for future studies to assess the exposure to BPA, NP, and OP in the general population.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
Glycosylation of the Fc region of IgG has a profound impact on the safety and clinical efficacy of therapeutic antibodies. While the biantennary complex.type oligosaccharide attached to Asn297 of the Fc is essen- tial...Glycosylation of the Fc region of IgG has a profound impact on the safety and clinical efficacy of therapeutic antibodies. While the biantennary complex.type oligosaccharide attached to Asn297 of the Fc is essen- tial for antibody effector functions, fucose and outer-arm sugars attached to the core heptasaccharide that gen- erate structural heterogeneity (glycoforms) exhibit unique biological activities. Hence, efficient and quan- titative glycan analysis techniques have been increas- ingly important for the development and quality control of therapeutic antibodies, and g|ycan profiles of the Fc are recognized as critical quality attributes. In the past decade our understanding of the influence of glycosy- lation on the structure/function of IgG-Fc has grown rapidly through X-ray crystallographic and nuclear magnetic resonance studies, which provides possibili- ties for the design of novel antibody therapeutics. Fur- thermore, the chemoenzymatic glycoengineering approach using endoglycosidase-based glycosyn- thases may facilitate the development of homogeneous IgG glycoforms with desirable functionality as next- generation therapeutic antibodies. Thus, the Fc glycans are fertile ground for the improvement of the safety,functionality, and efficacy of therapeutic IgG antibodies in the era of precision medicine.展开更多
Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in sur...Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in surface and tap water samples from 12 sites around Lake Taihu near Shanghai City in East China.Predominant PFCs were perfluorooctanoic acid(PFOA)and perfluorooctane sulfonate(PFOS),of which the concentration ranges were 6.8–206 and 1.2–45 ng·L^(–1),the geometric means were 35.3 and 9.4 ng·L^(–1),and the median(quartile range)values were 31.4(34.4)and 10.4(10.7)ng·L^(–1),respectively.Other PFCs were also detected but in much lower concentrations than PFOA.The sources of the PFCs were expected to be direct industrial discharges in the Lake Taihu area,and this area was also a possible source of PFCs contaminations in Shanghai district in the downstream.PFCs distributions were found different in the upstream,downstream and north part of Lake Taihu.Occurrences of PFCs in the tap water in Lake Taihu area indicated their exposure to the local people.A brief estimation of the environmental risks by PFCs implied no acute or immediate risks from PFCs to local human health,but chronic risks from PFOA in the tap water should be considered in the downstream regions.展开更多
文摘An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
基金supported by the Natural Science Foundation of Zhejiang Province,China(No.LY17C200009)the Foundation of Zhejiang Educational Committee(No.Y201328477)
文摘A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.
基金Supported by the National Natural Science Foundation of China(No.30901891)
文摘Objectives: To study the characteristics of serum metabonomics in coronary heart disease (CHD) patients diagnosed as phlegm or blood stasis pattern and explore effects of formula-pattern correspondence treatment. Methods: A total of 102 stable CHD patients were enrolled and divided into phlegm group (P group, n=52) and blood stasis group (BS group, n=50) according to pattern identification. Gualou Xiebai Banxia Decoction (瓜萎薤白半夏汤, GXBD) and Xuefu Zhuyu Decoction (血府逐瘀汤, XZD) were used as drug interventions. Relevant indicators of metabonomics were observed by ultra performance liquid chromatography mass spectrometry (UPLC-MS) and pattern recognition. Results: Levels of amino acids and phosphatidylethanolamine (PE) in the CHD group were much higher than those in healthy control group, while the levels of unsaturated fatty acids, sphingosine, Lyso, phosphatidylcholine (PC) were significantly lower (P〈0.01). Most of the differential metabolites between the CHD and the healthy groups were also common metabolites of phlegm and blood stasis. 7(Z), 10(Z)- hexadecadienoic acid and DPA were decreased in the P group and increased in the BS group. According to the quantity of retraced metabolites, improvement in metabonomics by formula-pattern correspondence was superior to that without correspondence in the BS group. Based on the varieties of metabolites, GXBD could improve the levels of docosapentaenoic acid (DPA), sphingomyelin (SM) (d34:1), and L-Lactic acid and XZD could ameliorate the levels of sphingosine and Vit E in the P group, in the BS group, GXBD could improve vitamin E level and XZD could make improvements in the levels of octadecanoic acid, phosphoglycerol, and SM (d34:1). Conclusions: Phlegm and blood stasis in CHD patients present specific differential metabolites, and share common metabolites. Remarkable differences have been displayed in pathological properties and severity of phlegm and blood stasis. Patients with phlegm are more likely to have lipid metabolism disorders. However, in patients with blood stasis, problems mainly lie in glucose, protein and fat metabolism and the injury of vascular cell membrane is relatively severe. The metabolic disorder is more complicated in blood stasis pattem than that in phlegm pattem. Compared with non-correspondence, improvement of differential metabolites is more comprehensive and targeted in formulapattern correspondence with a better effect.
文摘A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS) method was developed for the analysis of tetracycline antibiotics, including tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and their 4-epimers (4-epiTCs) in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution (pH 4.0), then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2:15:83 (v/v/v). The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method (LODsoil) ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.
基金Supported by the Fund for Key Labo ratory of Traditional Chinese Medicine Gan of State Administration of Traditional Chinese Medicinethe Major Research Plan of the National Natural Science Foundation of China(No.90409010)was partly supported by the Huge Project to Boost Chinese Drug Development(No.2009ZX09304-003)
文摘Objective: To detect absorbed bioactive compounds of the water extract whose pharmacodynamic effect was craniocerebral protection for quality control assessment. Methods: Anthraquinones in water extract of rhubarb (WER), in cerebrospinal fluid (CSF) of patients with traumatic brain injury (TBI) and in ipsilateral cortex of TBI rats following oral WER were respectively explored by ultra performance liquid chromatography with photodiode array detector (UPLC-PDA) method developed in the present study. The effects of anthraquinones absorbed into injured cortex on superoxidase dismutase (SOD) activity in TBI rats were detected. The antioxidative anthraquinones absorbed into target organ were evaluated for quality control of WER. Results: Anthraquinones in WER were aloe-emodin, rhein, emodin, chrysophanol, and physcion. Only the last anthraquinone was found in CSF and in ipsilateral cortex under this chromatographic condition. Physcion increased SOD activity in TBI rats significantly. Conclusions: Physcion was the main active compound of rhubarb against craniocerebral injury via antioxidant pathway. According to our strategy, the exploration of physcion suggested the possibility of a novel quality control of WER in treating TBI injury.
基金Supported by the Special Fund for Basic Scientific Research of Central Colleges,South-Central University for Nationalities(CZW15088)
文摘The enantiomer residues of metalaxyl, napropamide, triticonazole and metconazole were detected in soil by Qu EChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The soil sample was extracted with acetonitrile containing 1% acetic acid and purified using Qu ECh ERS method. Quantitative analysis for the enantiomers of these four chiral pesticides was performed in MS in multi-response monitoring(MRM) mode by external standard method. All enantiomers showed good linearity in the range of 0.5 to 50 μg/L. The average recoveries of enantiomers in soil were 81.74% to 105.79% with relative standard deviations(RSDs) from 3.69% to 7.86%. The method quantitative limit(MQL) was 5.3-30.3 ng/kg. The method can be used for rapid screening and determination of chiral pesticides in soil.
基金funded by the National Natural Science Foundation of China (40730740 & 20921063)the National Basic Research Program of China (2009CB421603)
文摘A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in negative mode. Plant samples were extracted and cleaned up through florisil column, resolved on a 100 mm C18 column with linear gradient elution and detected by mass spectrometry in multiple reaction monitoring (MRM) mode. The method provided good recoveries rang- ing from 68.2% to 94.6%, relative standard deviation (RSD) in the range of 3.2% - 9.1%, and limits of quantification (LOQ) defined as the signal-to-noise ratio of 10 of 0.3-2.1 ng/g. It allowed a fast separation and sensitive quantification of the isomers and homologues of seven OH-PBDE congeners 2′-OH-BDE-3, 3′-OH-BDE-7, 4′-OH-BDE-17, 3′-OH-BDE-28, 3-OH-BDE-47, 5-OH-BDE-47 and 6-OH-BDE-47. The method was successfully applied to identify and quantify the formation of hydroxylat- ed metabolites in alfalfa exposed to BDE-209. Five OH-PBDEs were detected in plant tissues, and more congeners were found in roots than in shoots. To our knowledge, this work represents the first attempt to validate UPLC-MS/MS method to quantify OH-PBDEs in plant samples without derivatization.
基金Supported by the National Key Research and Development Program of China(No.2016YFF0201104)the Construction of Public Service Platform for Research and Test of Marine Pilot Technology of China(No.Bhsfs009)the Project of Xiamen Southern oceanographic Center,China(No.16PFW008SF15).
文摘A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.
基金partly supported by National Natural Science Foundation of China(No.81430095)also by Special National Program on Key Basic Research Project(No.2014CB560706)
文摘Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after
基金Supported by Tongren Science and Technology Planning Project(TSKY[2022]42)Science Planning Project of Department of Education of Guizhou Province(2023B111)。
文摘[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value.
文摘The method of simultaneous analysis of Sudan Red Ⅰ-Ⅳ residues in ketchup was developed with an ultra performance liquid chromatography-tandem mass spectrum.Acetonitrile was used to extract the substance from the ketchup,and the upper layer was detected by the UPLC-MS/MS after refrigeration and centrifuge.The sample was separated on a Waters Acquity BHE C18 column,and detected by the MRM mode of the mass spectrum.The LOD was 2 ng/mL and the LOQ was 5 ng/mL all of the four substances.The average recoveries were between 67.42%-84.59% of the 100,200,300 μg/kg three spiked concentration levels and the RSD values were between 2.87%-9.57%.
文摘An ultra performance liquid chromatography-tandem mass spectrum method has been developed for the determination of three aconitum alkaloids (aconitine,hypaconitine and mesaconitine).The three alkaloids were analyzed simultaneously with an Waters Acquity BHE C18 column by gradient elution using 0.05% aqueous ammonia-acetonitrile as mobile phase and detected by the MRM mode of the mass spectrum.The recoveries of the SPE method were between 68.79%-95.65% (RSD<7.94%,n=4),and all the alkaloids showed good linearity (r>0.998) in a relatively wide concentration range.The LOD reached 0.0516,0.0640,0.0744 ng/mL of aconitine,hypaconitine and mesaconitine,respectively.The analysis time was within 3 min which could meet the high-throughput detection.The results indicated that contents of alkaloids in animal blood can be well detected;and this method can be used in quality control of aconitum drugs and pharmacokinetics study.
文摘Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of parathyroid hormone (PTH) in presence of meta-cresol as a stabilizer in a pharmaceutical formulation.Chromatography was performed with mobile phase containing 0.1% Trifluoroacetic acid (TFA) in MilliQ water and 0.1% TFA in acetonitrile with gradient program and flow rate at 0.3 mL/min for HPLC and 0.4 mL/min for UPLC.Quantification was accomplished with internal reference standard (qualified against innovator product and National Institute for Biological Standards and Control (NIBSC) standard).The methods were validated for linearity (correlation coefficient 0.99),range,accuracy,precision and robustness.Robustness was confirmed by considering three factors;mobile phase composition,column temperature and flow rate/age of mobile phase.Intermediate precision was confirmed on different equipments,different columns and on different days.The relative standard deviation (RSD) (<2% for RP-HPLC and <1% for UPLC,n=30) indicated a good precision.Retention time was found about 17 min and 2 min by HPLC and UPLC methods,respectively.Both methods are simple,highly sensitive,precise and accurate and have the potential of being useful for routine quality control.
基金Project of Traditional Chinese Medicine Administration of Guangxi Zhuang Autonomous Region(GZZC2019147)Project for Improving Basic Research Ability of Middle Aged and Young Teachers in Colleges and Universities of Guangxi in 2020(2020KY13034)+2 种基金The First Batch High-level Talent Scientific Research Project of The Affiliated Hospital of Youjiang Medical University for Nationalities in 2019(Y20196311)National Traditional Chinese Medicine Characteristic Technology Heritage Talent Training Program(2015481601003)Program of Youjiang Medical University for Nationalities(yy2018ky018).
文摘[Objectives]To establish a UPLC-UV method for the determination of polydatin in the serum of Wistar rats.[Methods]Acquity UPLC BEH shield RP18 column(1.7μm,2.1 mm×100 mm,Waters Corporation,USA)was used as the analytical column,acetonitrile-water(55∶45)was used as the mobile phase,the flow rate was 0.5 mL/min,and the column temperature was 30℃and the detection wavelength was 306 nm.[Results]The linear range of the established serum sample analysis method was 1.0-20.0μg/mL,and the correlation coefficient was r=0.9994;the intraday and interday RSD of Wistar rat serum was less than 3.0%,and the accuracy was higher than 90%.[Conclusions]This method is sensitive,accurate,and rapid.It is suitable for monitoring the concentration of polydatin in serum after intragastric administration,and can also be used for pharmacokinetics and bioavailability studies.
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supported by the National Science and Technology Fundation as par of the Key Technologies of Food Safety Project. Chemical pollutants exposure assessment technology research(2006BAK02A01)
文摘Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A (BPA), nonylphenol (NP), and octylphenol (OP) in urine samples. Methods Sixty urine samples collected from healthy subjects were analyzed for BPA, NP, and OP concentrations. The samples were de‐conjugated by adding β‐glucuronidase and sulfatase. After the enzymatic treatment, the samples were subjected to the OASIS HLB column solid phase extraction cartridges so as to be cleaned and concentrated. The UPLC separation was performed on a Acquity UPLCTM BEH C18 column (2.1×100 mm, 1.7 μm) with a gradient elution system of methanol‐water as the mobile phase. Triple‐quadrupole mass spectrometry analyzer was used for the qualitative and quantitative analysis of UPLC‐MS/MS system. Results The limit of detection of BPA, NP, and OP was 0.10, 0.10, and 0.15 ng/mL, respectively. The recoveries of BPA, NP and OP were 80.1%‐108%, 81.3%‐109%, and 81.5%‐98.7%, respectively. Among the 60 urine samples, BPA was detected in 8 samples at the level of 0.297‐32.7ng/mL, NP was detected in 29 samples at the level of 1.69‐27.8 ng/mL, and OP was detected in 17 samples at the level of 0.407‐11.1 ng/mL. Conclusion The method is simple with high sensitivity and selectivity, and is suitable for the determination of BPA, NP, and OP in urine. As shown by our analysis , BPA, NP, and OP appear to be prevalent in human urine. This is particularly true for NP. The results from our study is therefore valuable for future studies to assess the exposure to BPA, NP, and OP in the general population.
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.
文摘Glycosylation of the Fc region of IgG has a profound impact on the safety and clinical efficacy of therapeutic antibodies. While the biantennary complex.type oligosaccharide attached to Asn297 of the Fc is essen- tial for antibody effector functions, fucose and outer-arm sugars attached to the core heptasaccharide that gen- erate structural heterogeneity (glycoforms) exhibit unique biological activities. Hence, efficient and quan- titative glycan analysis techniques have been increas- ingly important for the development and quality control of therapeutic antibodies, and g|ycan profiles of the Fc are recognized as critical quality attributes. In the past decade our understanding of the influence of glycosy- lation on the structure/function of IgG-Fc has grown rapidly through X-ray crystallographic and nuclear magnetic resonance studies, which provides possibili- ties for the design of novel antibody therapeutics. Fur- thermore, the chemoenzymatic glycoengineering approach using endoglycosidase-based glycosyn- thases may facilitate the development of homogeneous IgG glycoforms with desirable functionality as next- generation therapeutic antibodies. Thus, the Fc glycans are fertile ground for the improvement of the safety,functionality, and efficacy of therapeutic IgG antibodies in the era of precision medicine.
基金the National Science and Technology Pillar Program of China(Grant No.2006BAC19B06)the Major Projects on Control and Rectification of Water Body Pollution(2009ZX07313-003).
文摘Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in surface and tap water samples from 12 sites around Lake Taihu near Shanghai City in East China.Predominant PFCs were perfluorooctanoic acid(PFOA)and perfluorooctane sulfonate(PFOS),of which the concentration ranges were 6.8–206 and 1.2–45 ng·L^(–1),the geometric means were 35.3 and 9.4 ng·L^(–1),and the median(quartile range)values were 31.4(34.4)and 10.4(10.7)ng·L^(–1),respectively.Other PFCs were also detected but in much lower concentrations than PFOA.The sources of the PFCs were expected to be direct industrial discharges in the Lake Taihu area,and this area was also a possible source of PFCs contaminations in Shanghai district in the downstream.PFCs distributions were found different in the upstream,downstream and north part of Lake Taihu.Occurrences of PFCs in the tap water in Lake Taihu area indicated their exposure to the local people.A brief estimation of the environmental risks by PFCs implied no acute or immediate risks from PFCs to local human health,but chronic risks from PFOA in the tap water should be considered in the downstream regions.