Compared to their linear counterparts,cyclic peptides show better biological activities,such as antibacterial,immunosuppressive,and anti-tumor activities,and pharmaceutical properties due to their conformational rigid...Compared to their linear counterparts,cyclic peptides show better biological activities,such as antibacterial,immunosuppressive,and anti-tumor activities,and pharmaceutical properties due to their conformational rigidity.However,cyclic peptides could form numerous putative metabolites from potential hydrolytic cleavages and their fragments are very difficult to interpret.These characteristics pose a great challenge when analyzing metabolites of cyclic peptides by mass spectrometry.This study was to assess and apply a software-aided analytical workflow for the detection and structural characterization of cyclic peptide metabolites.Insulin and atrial natriuretic peptide(ANP)as model cyclic peptides were incubated with trypsin/chymotrypsin and/or rat liver S9,followed by data acquisition using TripleTOF?5600.Resultant full-scan MS and MS/MS datasets were automatically processed through a combination of targeted and untargeted peak finding strategies.MS/MS spectra of predicted metabolites were interrogated against putative metabolite sequences,in light of a,b,y and internal fragment series.The resulting fragment assignments led to the confirmation and ranking of the metabolite sequences and identification of metabolic modification.As a result,29 metabolites with linear or cyclic structures were detected in the insulin incubation with the hydrolytic enzymes.Sequences of twenty insulin metabolites were further determined,which were consistent with the hydrolytic sites of these enzymes.In the same manner,multiple metabolites of insulin and ANP formed in rat liver S9 incubation were detected and structurally characterized,some of which have not been previously reported.The results demonstrated the utility of software-aided data processing tool in detection and identification of cyclic peptide metabolites.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
A single and dual parameter data acquisition, ion beam measurements and control system for accelerator mass spectrometry is described. The system hardware has been constructed with the advantage of the lower cost and ...A single and dual parameter data acquisition, ion beam measurements and control system for accelerator mass spectrometry is described. The system hardware has been constructed with the advantage of the lower cost and higher reliability. It is provided with varieties of functions such as selecting acquisition mode carrying out the multiple display, analyzing data and especially viewing isometric spectrum at different directions. It can also be used for ordinary nuclear spectrum system.展开更多
Liquid chromatography coupled to high resolution mass spectrometry(LC-HRMS)was used to establish a high throughput and sensitive method for 18 phthalic acid esters(PAEs)in textiles.The method was applied to screen PAE...Liquid chromatography coupled to high resolution mass spectrometry(LC-HRMS)was used to establish a high throughput and sensitive method for 18 phthalic acid esters(PAEs)in textiles.The method was applied to screen PAEs in 413 textile samples and 7 434 pieces of test data were analyzed.Further discussion was conducted about specific compounds,textile materials,detected value distribution and positive rate of samples.Twenty-nine percent of samples were detected with PAEs,and no samples were detected beyond regulations.Diisobutyl phthalate(DiBP),Dibutyl phthalate(DBP)and Di-2-ethylhexyl phthalate(DEHP)were detected with high frequency,and most samples were fabrics with coating and printing.This study can be used to reflect distribution of phthalate residues in textiles on the market and provide data support for risk assessment of PAEs for textile producers and consumers.展开更多
A real doping case for which the national-level reviewing body deemed it probable that a misidentification of the national-level athlete’s sample occurred at the WADA accredited laboratory, thus making the athlete in...A real doping case for which the national-level reviewing body deemed it probable that a misidentification of the national-level athlete’s sample occurred at the WADA accredited laboratory, thus making the athlete in this case strictly anonymous, is used to discuss criteria for data reduction and tolerance windows in GC-MS and LC-MS/MS. Stricter criteria for data reduction would remedy the present ambiguities.展开更多
The article evaluated the degradation of the captopril in aqueous solution after ozonation and chlorination. The process was continuously monitored focusing on the identification, mass spectrometry and elucidation of ...The article evaluated the degradation of the captopril in aqueous solution after ozonation and chlorination. The process was continuously monitored focusing on the identification, mass spectrometry and elucidation of its by-products by applying direct infusion and high performance liquid chromatography, electrospray ionization high resolution mass spectrometry, in the negative ion mode. The cytotoxicity of its by-products solutions were evaluated with 3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay. It was observed through that after 30 min of ozonation and chlorination, there was complete oxidation of captopril, i.e., 100% removal efficiency. At these conditions, the rate of mineralization, by total organic carbon, was only 7.63% for ozonation and 6.40% for chlorination, evidencing the formation of degradation by-products. Ten captopril by-products were identified and their respective chemical structures elucidations are proposed. The treated samples and their by-products were nontoxic to HepG2 cells by MTT assay.展开更多
Natural medicines(NMs)are crucial for treating human diseases.Efficiently characterizing their bioactive components in vivo has been a key focus and challenge in NM research.High-performance liquid chromatography-high...Natural medicines(NMs)are crucial for treating human diseases.Efficiently characterizing their bioactive components in vivo has been a key focus and challenge in NM research.High-performance liquid chromatography-high-resolution mass spectrometry(HPLC-HRMS)systems offer high sensitivity,resolution,and precision for conducting in vivo analysis of NMs.However,due to the complexity of NMs,conventional data acquisition,mining,and processing techniques often fail to meet the practical needs of in vivo NM analysis.Over the past two decades,intelligent spectral data-processing techniques based on various principles and algorithms have been developed and applied for in vivo NM analysis.Consequently,improvements have been achieved in the overall analytical performance by relying on these techniques without the need to change the instrument hardware.These improvements include enhanced instrument analysis sensitivity,expanded compound analysis coverage,intelligent identification,and characterization of nontargeted in vivo compounds,providing powerful technical means for studying the in vivo metabolism of NMs and screening for pharmacologically active components.This review summarizes the research progress on in vivo analysis strategies for NMs using intelligent MS data processing techniques reported over the past two decades.It discusses differences in compound structures,variations among biological samples,and the application of artificial intelligence(AI)neural network algorithms.Additionally,the review offers insights into the potential of in vivo tracking of NMs,including the screening of bioactive components and the identification of pharmacokinetic markers.The aim is to provide a reference for the integration and development of new technologies and strategies for future in vivo analysis of NMs.展开更多
To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectro...To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectrometry (HR-TOF/MS) with colorized fuzzy difference (CFD) method was used to investigate the effect of sulfur-fumigation on the volatile components from Radix Angelicae Sinensis. Twenty-five compounds that were found in sun-dried samples disappeared in sulfur-fumigated samples. Seventeen volatile components including two sulfur-containing compounds were newly generated for the first time in volatile oils of sulfur-fumigated Radix Angelicae Sinensis. The strategy can be successfully applied to rapidly and holistically discriminate sun-dried and sulfur-fumigated Radix Angelicae Sinensis. GCxGC-HR-TOF/MS based CFD is a powerful and feasible approach for the global quality evaluation of Radix Angelicae Sinensis as well as other herbal medicines.展开更多
依据专家感官审评结果将14个红茶样本按香气品质的优劣划分为优质红茶与缺陷红茶2组,基于快速气相电子鼻(fast gas chromatography-electronic-nose,GC-E-Nose)和气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)融合技术结...依据专家感官审评结果将14个红茶样本按香气品质的优劣划分为优质红茶与缺陷红茶2组,基于快速气相电子鼻(fast gas chromatography-electronic-nose,GC-E-Nose)和气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)融合技术结合多元统计分析对2组茶样进行判别分析,筛选影响两类茶样分类的关键差异组分。结果显示:GC-E-Nose(44维)和GC-MS(73维)相融合可以得到117维融合数据集,用其建立的正交偏最小二乘判别分析模型可以实现两类红茶的准确分类,其模型解释能力和预测能力(R_(Y)^(2)=0.976,Q^(2)=0.959)较单一的GC-E-Nose或GC-MS数据模型更优。基于变量投影重要性>1.6和P<0.05双变量原则,共筛选出二甲基硫醚(B3、B25)、β-紫罗酮(A59)、(3E)-4,8-二甲基壬-1,3,7-三烯(A20)、二氢猕猴桃内酯(A64)、芳樟醇(A17)、苯乙醇(A19)、δ-辛内酯(A41)和γ-壬内酯(A45)8个关键香气组分对分类起重要作用。研究结果表明,GC-E-Nose与GC-MS融合技术可以实现缺陷红茶和优质红茶的快速、准确分类,该方法可作为传统感官审评方法的补充,为红茶品质控制和质量提升提供技术支撑。展开更多
Ensuring the health and safety of drinking water is crucial for both nations and their citizens.Since the 20th century,the disinfection of drinking water,effectively controlling pathogens in water sources,has become o...Ensuring the health and safety of drinking water is crucial for both nations and their citizens.Since the 20th century,the disinfection of drinking water,effectively controlling pathogens in water sources,has become one of the significant advances in public health.However,the disinfectants used in the process,such as chlorine and chlorine dioxide,react with natural organic matter in the water to produce disinfection by-products(DBPs).Most of these DBPs contain chlorine,and if the source water contains bromine or iodine,brominated or iodinated DBPs,collectively referred to as Halogenated disinfection byproducts(X-DBPs),are formed.Numerous studies have found that X-DBPs pose potential risks to human health and the environment,leading to widespread concern.Mass spectrometry has become an important means of discovering new types of X-DBPs.This paper focuses on the study of methods for analyzing X-DBPs in drinking water using mass spectrometry.展开更多
A novel study using LCeMS(Liquid chromatography tandem mass spectrometry)coupled with multivariate data analysis and bioactivity evaluation was established for discrimination of aqueous extract and vinegar extract of...A novel study using LCeMS(Liquid chromatography tandem mass spectrometry)coupled with multivariate data analysis and bioactivity evaluation was established for discrimination of aqueous extract and vinegar extract of Shixiao San.Batches of these two kinds of samples were subjected to analysis,and the datasets of sample codes,tR-m/z pairs and ion intensities were processed with principal component analysis(PCA).The result of score plot showed a clear classification of the aqueous and vinegar groups.And the chemical markers having great contributions to the differentiation were screened out on the loading plot.The identities of the chemical markers were performed by comparing the mass fragments and retention times with those of reference compounds and/or the known compounds published in the literatures.Based on the proposed strategy,quercetin-3-Oneohesperidoside,isorhamnetin-3-O-neohespeeridoside,kaempferol-3-O-neohesperidoside,isorhamnetin-3-O-rutinoside and isorhamnetin-3-O-(2G-a-l-rhamnosyl)-rutinoside were explored as representative markers in distinguishing the vinegar extract from the aqueous extract.The anti-hyperlipidemic activities of two processed extracts of Shixiao San were examined on serum levels of lipids,lipoprotein and blood antioxidant enzymes in a rat hyperlipidemia model,and the vinegary extract,exerting strong lipid-lowering and antioxidative effects,was superior to the aqueous extract.Therefore,boiling with vinegary was predicted as the greatest processing procedure for anti-hyperlipidemic effect of Shixiao San.Furthermore,combining the changes in the metabolic profiling and bioactivity evaluation,the five representative markers may be related to the observed antihyperlipidemic effect.展开更多
Volatile nitrosamines (VNAs) are a group of compounds classified as probable (group 2A) and possible (group 2B) carcinogens in humans. Along with certain foods and contaminated drinking water, VNAs are detected at hig...Volatile nitrosamines (VNAs) are a group of compounds classified as probable (group 2A) and possible (group 2B) carcinogens in humans. Along with certain foods and contaminated drinking water, VNAs are detected at high levels in tobacco products and in both mainstream and side-stream smoke. Our laboratory monitors six urinary VNAs—N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopiperidine (NPIP), N-nitrosopyrrolidine (NPYR), and N-nitrosomorpholine (NMOR)—using isotope dilution GC-MS/ MS (QQQ) for large population studies such as the National Health and Nutrition Examination Survey (NHANES). In this paper, we report for the first time a new automated sample preparation method to more efficiently quantitate these VNAs. Automation is done using Hamilton STAR<sup>TM</sup> and Caliper Staccato<sup>TM</sup> workstations. This new automated method reduces sample preparation time from 4 hours to 2.5 hours while maintaining precision (inter-run CV < 10%) and accuracy (85% - 111%). More importantly this method increases sample throughput while maintaining a low limit of detection (<10 pg/mL) for all analytes. A streamlined sample data flow was created in parallel to the automated method, in which samples can be tracked from receiving to final LIMs output with minimal human intervention, further minimizing human error in the sample preparation process. This new automated method and the sample data flow are currently applied in bio-monitoring of VNAs in the US non-institutionalized population NHANES 2013-2014 cycle.展开更多
文摘Compared to their linear counterparts,cyclic peptides show better biological activities,such as antibacterial,immunosuppressive,and anti-tumor activities,and pharmaceutical properties due to their conformational rigidity.However,cyclic peptides could form numerous putative metabolites from potential hydrolytic cleavages and their fragments are very difficult to interpret.These characteristics pose a great challenge when analyzing metabolites of cyclic peptides by mass spectrometry.This study was to assess and apply a software-aided analytical workflow for the detection and structural characterization of cyclic peptide metabolites.Insulin and atrial natriuretic peptide(ANP)as model cyclic peptides were incubated with trypsin/chymotrypsin and/or rat liver S9,followed by data acquisition using TripleTOF?5600.Resultant full-scan MS and MS/MS datasets were automatically processed through a combination of targeted and untargeted peak finding strategies.MS/MS spectra of predicted metabolites were interrogated against putative metabolite sequences,in light of a,b,y and internal fragment series.The resulting fragment assignments led to the confirmation and ranking of the metabolite sequences and identification of metabolic modification.As a result,29 metabolites with linear or cyclic structures were detected in the insulin incubation with the hydrolytic enzymes.Sequences of twenty insulin metabolites were further determined,which were consistent with the hydrolytic sites of these enzymes.In the same manner,multiple metabolites of insulin and ANP formed in rat liver S9 incubation were detected and structurally characterized,some of which have not been previously reported.The results demonstrated the utility of software-aided data processing tool in detection and identification of cyclic peptide metabolites.
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.
文摘A single and dual parameter data acquisition, ion beam measurements and control system for accelerator mass spectrometry is described. The system hardware has been constructed with the advantage of the lower cost and higher reliability. It is provided with varieties of functions such as selecting acquisition mode carrying out the multiple display, analyzing data and especially viewing isometric spectrum at different directions. It can also be used for ordinary nuclear spectrum system.
基金National Key R&D Program of China(No.2016YFF0203702)Quality Inspection Public Welfare Scientific Research Foundation of China(No.201310062)Science Research Program of General Administration of Quality Supervision,Inspection and Quarantine of China(No.2011IK037)
文摘Liquid chromatography coupled to high resolution mass spectrometry(LC-HRMS)was used to establish a high throughput and sensitive method for 18 phthalic acid esters(PAEs)in textiles.The method was applied to screen PAEs in 413 textile samples and 7 434 pieces of test data were analyzed.Further discussion was conducted about specific compounds,textile materials,detected value distribution and positive rate of samples.Twenty-nine percent of samples were detected with PAEs,and no samples were detected beyond regulations.Diisobutyl phthalate(DiBP),Dibutyl phthalate(DBP)and Di-2-ethylhexyl phthalate(DEHP)were detected with high frequency,and most samples were fabrics with coating and printing.This study can be used to reflect distribution of phthalate residues in textiles on the market and provide data support for risk assessment of PAEs for textile producers and consumers.
文摘A real doping case for which the national-level reviewing body deemed it probable that a misidentification of the national-level athlete’s sample occurred at the WADA accredited laboratory, thus making the athlete in this case strictly anonymous, is used to discuss criteria for data reduction and tolerance windows in GC-MS and LC-MS/MS. Stricter criteria for data reduction would remedy the present ambiguities.
基金the Minas Gerais State Science Foundation(FAPEMIG)-process APQ-00918-13the Brazilian National Research Council(CNPq)-process 473893-2013-1 for their financial support and the granting of research fellowships.
文摘The article evaluated the degradation of the captopril in aqueous solution after ozonation and chlorination. The process was continuously monitored focusing on the identification, mass spectrometry and elucidation of its by-products by applying direct infusion and high performance liquid chromatography, electrospray ionization high resolution mass spectrometry, in the negative ion mode. The cytotoxicity of its by-products solutions were evaluated with 3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) assay. It was observed through that after 30 min of ozonation and chlorination, there was complete oxidation of captopril, i.e., 100% removal efficiency. At these conditions, the rate of mineralization, by total organic carbon, was only 7.63% for ozonation and 6.40% for chlorination, evidencing the formation of degradation by-products. Ten captopril by-products were identified and their respective chemical structures elucidations are proposed. The treated samples and their by-products were nontoxic to HepG2 cells by MTT assay.
基金supported by the National Natural Science Foundation of China(Nos.82222068,82141215 and 82173779)the Innovation Team and Talents Cultivation Program of National Administration of Traditional Chinese Medicine(No.ZYYCXTD-D-202206)+1 种基金the Science and Technology Project of Fujian Province(Nos.2022J02057,2021J02058 and 2021I0003)the S&T Program of Hebei Province(No.23372508D)。
文摘Natural medicines(NMs)are crucial for treating human diseases.Efficiently characterizing their bioactive components in vivo has been a key focus and challenge in NM research.High-performance liquid chromatography-high-resolution mass spectrometry(HPLC-HRMS)systems offer high sensitivity,resolution,and precision for conducting in vivo analysis of NMs.However,due to the complexity of NMs,conventional data acquisition,mining,and processing techniques often fail to meet the practical needs of in vivo NM analysis.Over the past two decades,intelligent spectral data-processing techniques based on various principles and algorithms have been developed and applied for in vivo NM analysis.Consequently,improvements have been achieved in the overall analytical performance by relying on these techniques without the need to change the instrument hardware.These improvements include enhanced instrument analysis sensitivity,expanded compound analysis coverage,intelligent identification,and characterization of nontargeted in vivo compounds,providing powerful technical means for studying the in vivo metabolism of NMs and screening for pharmacologically active components.This review summarizes the research progress on in vivo analysis strategies for NMs using intelligent MS data processing techniques reported over the past two decades.It discusses differences in compound structures,variations among biological samples,and the application of artificial intelligence(AI)neural network algorithms.Additionally,the review offers insights into the potential of in vivo tracking of NMs,including the screening of bioactive components and the identification of pharmacokinetic markers.The aim is to provide a reference for the integration and development of new technologies and strategies for future in vivo analysis of NMs.
基金Supported by the National Natural Science Foundation of China(No.81173546 and No.30940093)the Natural Science Foundation of Jiangsu Province,China(No.BK2009495)+4 种基金the International Science and Technology Cooperation Project of Jiangsu Province,China(No.BZ2011053)the Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions(PAPD,No.2011ZYX2-001)the Postgraduate Research Innovation Project of Jiangsu Higher Education Institutions(No.KYLX_0975)the Chinese Medicine Research Program of Zhejiang Province,China(No.2014ZQ008)the Science Foundation of Zhejiang Chinese Medical University(No.2013ZZ12)
文摘To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectrometry (HR-TOF/MS) with colorized fuzzy difference (CFD) method was used to investigate the effect of sulfur-fumigation on the volatile components from Radix Angelicae Sinensis. Twenty-five compounds that were found in sun-dried samples disappeared in sulfur-fumigated samples. Seventeen volatile components including two sulfur-containing compounds were newly generated for the first time in volatile oils of sulfur-fumigated Radix Angelicae Sinensis. The strategy can be successfully applied to rapidly and holistically discriminate sun-dried and sulfur-fumigated Radix Angelicae Sinensis. GCxGC-HR-TOF/MS based CFD is a powerful and feasible approach for the global quality evaluation of Radix Angelicae Sinensis as well as other herbal medicines.
文摘依据专家感官审评结果将14个红茶样本按香气品质的优劣划分为优质红茶与缺陷红茶2组,基于快速气相电子鼻(fast gas chromatography-electronic-nose,GC-E-Nose)和气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)融合技术结合多元统计分析对2组茶样进行判别分析,筛选影响两类茶样分类的关键差异组分。结果显示:GC-E-Nose(44维)和GC-MS(73维)相融合可以得到117维融合数据集,用其建立的正交偏最小二乘判别分析模型可以实现两类红茶的准确分类,其模型解释能力和预测能力(R_(Y)^(2)=0.976,Q^(2)=0.959)较单一的GC-E-Nose或GC-MS数据模型更优。基于变量投影重要性>1.6和P<0.05双变量原则,共筛选出二甲基硫醚(B3、B25)、β-紫罗酮(A59)、(3E)-4,8-二甲基壬-1,3,7-三烯(A20)、二氢猕猴桃内酯(A64)、芳樟醇(A17)、苯乙醇(A19)、δ-辛内酯(A41)和γ-壬内酯(A45)8个关键香气组分对分类起重要作用。研究结果表明,GC-E-Nose与GC-MS融合技术可以实现缺陷红茶和优质红茶的快速、准确分类,该方法可作为传统感官审评方法的补充,为红茶品质控制和质量提升提供技术支撑。
文摘Ensuring the health and safety of drinking water is crucial for both nations and their citizens.Since the 20th century,the disinfection of drinking water,effectively controlling pathogens in water sources,has become one of the significant advances in public health.However,the disinfectants used in the process,such as chlorine and chlorine dioxide,react with natural organic matter in the water to produce disinfection by-products(DBPs).Most of these DBPs contain chlorine,and if the source water contains bromine or iodine,brominated or iodinated DBPs,collectively referred to as Halogenated disinfection byproducts(X-DBPs),are formed.Numerous studies have found that X-DBPs pose potential risks to human health and the environment,leading to widespread concern.Mass spectrometry has become an important means of discovering new types of X-DBPs.This paper focuses on the study of methods for analyzing X-DBPs in drinking water using mass spectrometry.
基金Natural Science Foundation of China(T11036061/T0108).
文摘A novel study using LCeMS(Liquid chromatography tandem mass spectrometry)coupled with multivariate data analysis and bioactivity evaluation was established for discrimination of aqueous extract and vinegar extract of Shixiao San.Batches of these two kinds of samples were subjected to analysis,and the datasets of sample codes,tR-m/z pairs and ion intensities were processed with principal component analysis(PCA).The result of score plot showed a clear classification of the aqueous and vinegar groups.And the chemical markers having great contributions to the differentiation were screened out on the loading plot.The identities of the chemical markers were performed by comparing the mass fragments and retention times with those of reference compounds and/or the known compounds published in the literatures.Based on the proposed strategy,quercetin-3-Oneohesperidoside,isorhamnetin-3-O-neohespeeridoside,kaempferol-3-O-neohesperidoside,isorhamnetin-3-O-rutinoside and isorhamnetin-3-O-(2G-a-l-rhamnosyl)-rutinoside were explored as representative markers in distinguishing the vinegar extract from the aqueous extract.The anti-hyperlipidemic activities of two processed extracts of Shixiao San were examined on serum levels of lipids,lipoprotein and blood antioxidant enzymes in a rat hyperlipidemia model,and the vinegary extract,exerting strong lipid-lowering and antioxidative effects,was superior to the aqueous extract.Therefore,boiling with vinegary was predicted as the greatest processing procedure for anti-hyperlipidemic effect of Shixiao San.Furthermore,combining the changes in the metabolic profiling and bioactivity evaluation,the five representative markers may be related to the observed antihyperlipidemic effect.
文摘Volatile nitrosamines (VNAs) are a group of compounds classified as probable (group 2A) and possible (group 2B) carcinogens in humans. Along with certain foods and contaminated drinking water, VNAs are detected at high levels in tobacco products and in both mainstream and side-stream smoke. Our laboratory monitors six urinary VNAs—N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopiperidine (NPIP), N-nitrosopyrrolidine (NPYR), and N-nitrosomorpholine (NMOR)—using isotope dilution GC-MS/ MS (QQQ) for large population studies such as the National Health and Nutrition Examination Survey (NHANES). In this paper, we report for the first time a new automated sample preparation method to more efficiently quantitate these VNAs. Automation is done using Hamilton STAR<sup>TM</sup> and Caliper Staccato<sup>TM</sup> workstations. This new automated method reduces sample preparation time from 4 hours to 2.5 hours while maintaining precision (inter-run CV < 10%) and accuracy (85% - 111%). More importantly this method increases sample throughput while maintaining a low limit of detection (<10 pg/mL) for all analytes. A streamlined sample data flow was created in parallel to the automated method, in which samples can be tracked from receiving to final LIMs output with minimal human intervention, further minimizing human error in the sample preparation process. This new automated method and the sample data flow are currently applied in bio-monitoring of VNAs in the US non-institutionalized population NHANES 2013-2014 cycle.