目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测...目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测(MRM)模式下进行测定,内标法定量。结果 10种真菌毒素含量在各自质量浓度范围内具有较好的线性关系(r>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为83.8%~107.1%(RSD<6.5%),定量限(LOQ)为0.18~129μg/kg。结论 该法前处理步骤简便,净化效果良好,提高了样品检测效率,内标法定量精准可靠,适用于蜂房及其制剂中10种真菌毒素的同时检测。展开更多
New ionization and detection techniques in mass spectrometry have been successfully applied for efficient analyses of complex biological systems. It is, however, still difficult to trace structural changes of a specif...New ionization and detection techniques in mass spectrometry have been successfully applied for efficient analyses of complex biological systems. It is, however, still difficult to trace structural changes of a specific molecular species in such systems. In the present study, a molecular probe strategy in combination with tandem electrospray ionization mass spectrometry has been examined using synthetic deuterium-labeled phosphatidylcholine hydroperoxide (PC-OOH/D3) and ethyl-labeled phosphatidylcholine having docosahexaenoic acid side chain (DHA-PC/Et). Administration of a mixture of PC-OOH/D3 and DHA-PC/Et to human blood and human skin surface, followed by extraction and analysis with collision-induced tandem electrospray ionization mass spectrometry demonstrated that metabolites of both molecular probes can be detected simultaneously with strict selectivity. The present method is also found to be useful in tracing chemical changes of the unstable docosahexaenoyl group on the surface of processed fish. The activity of phospholipase A2 can also be assessed using a phospholipid molecular probe with a linoleoyl and a deuteriomethyl group via selective detection of the lyso-phospholipid product by mass spectrometry. The advantage of the present method is that no chromatographic separation is required and analysis can be performed under strictly the same condition for different molecular probes, affording multiple data by one experiment. The present strategy may be useful for tracing time-dependent phenomena in dynamic phospholipid biochemistry, and can be widely used for any biological and food systems.展开更多
The work demonstrates an example of application of ^252Cf PDMS （plasma desorption mass spectrometry） to analysis of lipid profile of carotene-containing Blakeslea trispora biomass. It was shown that this method allo...The work demonstrates an example of application of ^252Cf PDMS （plasma desorption mass spectrometry） to analysis of lipid profile of carotene-containing Blakeslea trispora biomass. It was shown that this method allows identification of the individual components in the crude multicomponent mixtures not subjected to previous chromatographic separation or enrichment. Using a very simple pretreatment by different extractants permits to select preferable lipid fractions of microorganisms.展开更多
AIM To identify the effects and mechanism of action of Polygonatum kingianum(P. kingianum) on dyslipidemia in rats using an integrated untargeted metabolomic method.METHODS A rat model of dyslipidemia was induced with...AIM To identify the effects and mechanism of action of Polygonatum kingianum(P. kingianum) on dyslipidemia in rats using an integrated untargeted metabolomic method.METHODS A rat model of dyslipidemia was induced with a high-fat diet(HFD) and rats were given P. kingianum [4 g/(kg·d)] intragastrically for 14 wk. Changes in serum and hepatic lipid parameters were evaluated. Metabolites in serum, urine and liver samples were profiled using ultra-highperformance liquid chromatography/mass spectrometry followed by multivariate statistical analysis to identify potential biomarkers and metabolic pathways.RESULTS P. kingianum significantly inhibited the HFD-induced increase in total cholesterol and triglyceride in the liver and serum. P. kingianum also significantly regulated metabolites in the analyzed samples toward normal status. Nineteen, twenty-four and thirty-eight potential biomarkers were identified in serum, urine and liver samples, respectively. These biomarkers involved biosynthesis of phenylalanine, tyrosine, tryptophan, valine, leucine and isoleucine, along with metabolism of tryptophan, tyrosine, phenylalanine, starch, sucrose, glycerophospholipid, arachidonic acid, linoleic acid, nicotinate, nicotinamide and sphingolipid.CONCLUSION P. kingianum alleviates HFD-induced dyslipidemia by regulating many endogenous metabolites in serum, urine and liver samples. Collectively, our findings suggest that P. kingianum may be a promising lipid regulator to treat dyslipidemia and associated diseases.展开更多
[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established acc...[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established according to Agilent Bond Elut enhanced lipid removal EMR-Lipid technology. [ Methods] Egg was extracted by acidified acetonitrile, purified by Bond Elut EMR-Lipid QuEChERS, and detected by HPLC-MS/MS. [ Results] The three kinds of polyether residues had good linear relationships in the range of 2.0 - 100 μg/L with peak areas, r 〉 0. 999. The recoveries ranged from 84.6% to 107.0%. [ Conclusions ] The method is convenient and accurate, and the quantitative results are accurate and reproducible. It is suitable for the determination of the three kinds of polyether residues in eggs.展开更多
目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,...目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,气相色谱-质谱联用仪多反应监测(multiple reaction monitoring,MRM)模式检测,采用基质匹配标准溶液内标法定量。结果218种农药在5~200 ng/mL范围内线性关系良好,相关系数均大于0.995,在0.05、0.10、0.50 mg/kg 3个添加水平的回收率为63.3%~119.9%,相对标准偏差(relative standard deviations,RSDs)为0.78%~18.10%,定量限(limits of the quantitation,LOQs)为10~20μg/kg。结论该方法前处理简单、高效,灵敏度、准确度和精密度高,能满足玉米油中218种农药多残留的分析要求。展开更多
Identification and quantification of lipids, in particular sphingolipids from intestine and liver, using multidimensional mass spectrometry has dramatically improved our understanding of lipid-based molecular pathways...Identification and quantification of lipids, in particular sphingolipids from intestine and liver, using multidimensional mass spectrometry has dramatically improved our understanding of lipid-based molecular pathways and signaling. The editorial gives a short overview about basic technical approaches to characterize lipids from intestine and liver.展开更多
The purpose of this preliminary study was to determine the comparative lipid profile of blood plasma samples of healthy individuals and patients with Myeloproliferative Neoplasms. Methods: Untargeted Shotgun MS/MS Ana...The purpose of this preliminary study was to determine the comparative lipid profile of blood plasma samples of healthy individuals and patients with Myeloproliferative Neoplasms. Methods: Untargeted Shotgun MS/MS Analysis was performed to evaluate plasma samples from 153 participants, being 90 of the Control Group, 43 Myeloproliferative Neoplasms (MPN), 11 Myelodysplastic Syndromes (MDS) and 9 Acute Myeloid Leukemias (AML). Lipids were extracted from plasma using the Bligh-Dyer protocol. Data were acquired using the AB-Sciex Analyst TF, processed using the AB-Sciex LipidViewTM and the web-based analytical pipeline MetaboAnalyst 2.0 (www.metaboanalyst.ca). Results: Untargeted analysis identified in negative and positive-modes a total of 658 features at 2 ppm resolution. PCA and PLS-DA analysis revealed clear discrimination among groups, in particular for AML patients. Main lipid groups differentially expressed were: Monoacylglycerols (MAG), Glucosylceramide E (GlcdE), Ethyl Esters (EE), Lysophosphatidic acid (LPA), Sulfoquinovosil diacylglycerols (SQDG), Monoglycerols (MG), Methyl Ethanolamines (ME), Lysophosphatidylcholines (LPC), Dimethyl Phosfatidyletanolamines (DMPE), Monometylphosphatidiletanolamines (MMPE), Ceramide-1-phosphate (CerP), Glicerophosphoglycerols (GP), Lysomonomethyl-Phosphatidylethanolamines (LMMPE), Phosphatidic Acids (PA), Ergosterols (ERG), Glycerophosphoserine (PS), Diacylglycerols (DAG), Hexocylceramides (HexCer) and Lanosterol (Lan). ROC Curve Analysis revealed Total LMMPE as the strongest discriminating marker between Controls from Patients. In addition, these lipids were also able to differentiate MDS and AML from NPM. Conclusions: The Myeloproliferative Neoplasms from the point of view of global plasma lipidomics are accompanied by several modifications. In particular, the Lysomonomethyl-Phosphatidylethanolamines (LMMPE) seems to play important differentiating roles among them.展开更多
The discipline of lipidomics, as coined in 2003, has made profound advances and been rapidly expanded. Direct infusion-based shotgun lipidomics contributes a major part of the research in this discipline. However, des...The discipline of lipidomics, as coined in 2003, has made profound advances and been rapidly expanded. Direct infusion-based shotgun lipidomics contributes a major part of the research in this discipline. However, despite of its numerous advantages over other lipidomics platforms, the classical shotgun lipidomics approach suffers ion suppression and has the difficulties to assess low abundance lipid classes, particularly those less ionizable or that do not yield sensitive and specific fragments. To overcome this obstacle and broaden coverage, strategies have been developed based on unique chemistry and/or physics of lipid classes of interest to enhance shotgun lipidomics. This article overviews the recent enhancements of shotgun lipidomics, including prefractionation, acid/base hydrolysis, derivatization, charge feature utilization. We believe that, by this versatile platform, comprehensive coverage of cellular lipidomes would be achieved in more accurate and effective manner. Therefore, application of the enhanced shotgun lipidomics would greatly accelerate lipidomics research to substantiate the aberrant lipid metabolism, signaling, trafficking, and homeostasis under pathological conditions and their underpinning biochemical mechanisms. It would also facilitate precision medicine studies.展开更多
文摘New ionization and detection techniques in mass spectrometry have been successfully applied for efficient analyses of complex biological systems. It is, however, still difficult to trace structural changes of a specific molecular species in such systems. In the present study, a molecular probe strategy in combination with tandem electrospray ionization mass spectrometry has been examined using synthetic deuterium-labeled phosphatidylcholine hydroperoxide (PC-OOH/D3) and ethyl-labeled phosphatidylcholine having docosahexaenoic acid side chain (DHA-PC/Et). Administration of a mixture of PC-OOH/D3 and DHA-PC/Et to human blood and human skin surface, followed by extraction and analysis with collision-induced tandem electrospray ionization mass spectrometry demonstrated that metabolites of both molecular probes can be detected simultaneously with strict selectivity. The present method is also found to be useful in tracing chemical changes of the unstable docosahexaenoyl group on the surface of processed fish. The activity of phospholipase A2 can also be assessed using a phospholipid molecular probe with a linoleoyl and a deuteriomethyl group via selective detection of the lyso-phospholipid product by mass spectrometry. The advantage of the present method is that no chromatographic separation is required and analysis can be performed under strictly the same condition for different molecular probes, affording multiple data by one experiment. The present strategy may be useful for tracing time-dependent phenomena in dynamic phospholipid biochemistry, and can be widely used for any biological and food systems.
文摘The work demonstrates an example of application of ^252Cf PDMS （plasma desorption mass spectrometry） to analysis of lipid profile of carotene-containing Blakeslea trispora biomass. It was shown that this method allows identification of the individual components in the crude multicomponent mixtures not subjected to previous chromatographic separation or enrichment. Using a very simple pretreatment by different extractants permits to select preferable lipid fractions of microorganisms.
基金Supported by the National Natural Science Foundation of China,No.81660596 and No.81760733the Application and Basis Research Project of Yunnan,China,No.2016FD050 and No.2017FF117-013the Fund for Young and Middle-aged Academic and Technological Leaders of Yunnan,No.2015HB053
文摘AIM To identify the effects and mechanism of action of Polygonatum kingianum(P. kingianum) on dyslipidemia in rats using an integrated untargeted metabolomic method.METHODS A rat model of dyslipidemia was induced with a high-fat diet(HFD) and rats were given P. kingianum [4 g/(kg·d)] intragastrically for 14 wk. Changes in serum and hepatic lipid parameters were evaluated. Metabolites in serum, urine and liver samples were profiled using ultra-highperformance liquid chromatography/mass spectrometry followed by multivariate statistical analysis to identify potential biomarkers and metabolic pathways.RESULTS P. kingianum significantly inhibited the HFD-induced increase in total cholesterol and triglyceride in the liver and serum. P. kingianum also significantly regulated metabolites in the analyzed samples toward normal status. Nineteen, twenty-four and thirty-eight potential biomarkers were identified in serum, urine and liver samples, respectively. These biomarkers involved biosynthesis of phenylalanine, tyrosine, tryptophan, valine, leucine and isoleucine, along with metabolism of tryptophan, tyrosine, phenylalanine, starch, sucrose, glycerophospholipid, arachidonic acid, linoleic acid, nicotinate, nicotinamide and sphingolipid.CONCLUSION P. kingianum alleviates HFD-induced dyslipidemia by regulating many endogenous metabolites in serum, urine and liver samples. Collectively, our findings suggest that P. kingianum may be a promising lipid regulator to treat dyslipidemia and associated diseases.
基金Supported by Science and Technology Planning Project of Huizhou City(20161117141959)
文摘[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established according to Agilent Bond Elut enhanced lipid removal EMR-Lipid technology. [ Methods] Egg was extracted by acidified acetonitrile, purified by Bond Elut EMR-Lipid QuEChERS, and detected by HPLC-MS/MS. [ Results] The three kinds of polyether residues had good linear relationships in the range of 2.0 - 100 μg/L with peak areas, r 〉 0. 999. The recoveries ranged from 84.6% to 107.0%. [ Conclusions ] The method is convenient and accurate, and the quantitative results are accurate and reproducible. It is suitable for the determination of the three kinds of polyether residues in eggs.
文摘目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,气相色谱-质谱联用仪多反应监测(multiple reaction monitoring,MRM)模式检测,采用基质匹配标准溶液内标法定量。结果218种农药在5~200 ng/mL范围内线性关系良好,相关系数均大于0.995,在0.05、0.10、0.50 mg/kg 3个添加水平的回收率为63.3%~119.9%,相对标准偏差(relative standard deviations,RSDs)为0.78%~18.10%,定量限(limits of the quantitation,LOQs)为10~20μg/kg。结论该方法前处理简单、高效,灵敏度、准确度和精密度高,能满足玉米油中218种农药多残留的分析要求。
文摘Identification and quantification of lipids, in particular sphingolipids from intestine and liver, using multidimensional mass spectrometry has dramatically improved our understanding of lipid-based molecular pathways and signaling. The editorial gives a short overview about basic technical approaches to characterize lipids from intestine and liver.
文摘The purpose of this preliminary study was to determine the comparative lipid profile of blood plasma samples of healthy individuals and patients with Myeloproliferative Neoplasms. Methods: Untargeted Shotgun MS/MS Analysis was performed to evaluate plasma samples from 153 participants, being 90 of the Control Group, 43 Myeloproliferative Neoplasms (MPN), 11 Myelodysplastic Syndromes (MDS) and 9 Acute Myeloid Leukemias (AML). Lipids were extracted from plasma using the Bligh-Dyer protocol. Data were acquired using the AB-Sciex Analyst TF, processed using the AB-Sciex LipidViewTM and the web-based analytical pipeline MetaboAnalyst 2.0 (www.metaboanalyst.ca). Results: Untargeted analysis identified in negative and positive-modes a total of 658 features at 2 ppm resolution. PCA and PLS-DA analysis revealed clear discrimination among groups, in particular for AML patients. Main lipid groups differentially expressed were: Monoacylglycerols (MAG), Glucosylceramide E (GlcdE), Ethyl Esters (EE), Lysophosphatidic acid (LPA), Sulfoquinovosil diacylglycerols (SQDG), Monoglycerols (MG), Methyl Ethanolamines (ME), Lysophosphatidylcholines (LPC), Dimethyl Phosfatidyletanolamines (DMPE), Monometylphosphatidiletanolamines (MMPE), Ceramide-1-phosphate (CerP), Glicerophosphoglycerols (GP), Lysomonomethyl-Phosphatidylethanolamines (LMMPE), Phosphatidic Acids (PA), Ergosterols (ERG), Glycerophosphoserine (PS), Diacylglycerols (DAG), Hexocylceramides (HexCer) and Lanosterol (Lan). ROC Curve Analysis revealed Total LMMPE as the strongest discriminating marker between Controls from Patients. In addition, these lipids were also able to differentiate MDS and AML from NPM. Conclusions: The Myeloproliferative Neoplasms from the point of view of global plasma lipidomics are accompanied by several modifications. In particular, the Lysomonomethyl-Phosphatidylethanolamines (LMMPE) seems to play important differentiating roles among them.
文摘The discipline of lipidomics, as coined in 2003, has made profound advances and been rapidly expanded. Direct infusion-based shotgun lipidomics contributes a major part of the research in this discipline. However, despite of its numerous advantages over other lipidomics platforms, the classical shotgun lipidomics approach suffers ion suppression and has the difficulties to assess low abundance lipid classes, particularly those less ionizable or that do not yield sensitive and specific fragments. To overcome this obstacle and broaden coverage, strategies have been developed based on unique chemistry and/or physics of lipid classes of interest to enhance shotgun lipidomics. This article overviews the recent enhancements of shotgun lipidomics, including prefractionation, acid/base hydrolysis, derivatization, charge feature utilization. We believe that, by this versatile platform, comprehensive coverage of cellular lipidomes would be achieved in more accurate and effective manner. Therefore, application of the enhanced shotgun lipidomics would greatly accelerate lipidomics research to substantiate the aberrant lipid metabolism, signaling, trafficking, and homeostasis under pathological conditions and their underpinning biochemical mechanisms. It would also facilitate precision medicine studies.
