Milk and dairy products are more and more popular with consumers due to their various nutrients, and their quality and safety issues have always been concerned. Therefore, the development of rapid, accurate and simple...Milk and dairy products are more and more popular with consumers due to their various nutrients, and their quality and safety issues have always been concerned. Therefore, the development of rapid, accurate and simple screening techniques is of great significance. Liquid chromatography-high resolution time-of-flight mass spectrometry has high-resolution and high-throughput detection functions, and has gradually begun to be applied in the detection of milk and dairy products. This paper summarized the application of milk and dairy products in liquid chromatography-high resolution time-of-flight mass spectrometry, laying a foundation for the development of new methods.展开更多
An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrome...An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis of the analysis of the first dimension, retention components of the urine sample were collected into 30 fractions （one fraction per minute）. Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine （Songorine, 14-benzoylneoline, Deoxyaconitine, etc. ） exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the system suggest that the CMC can be applied to in vivo study.展开更多
[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-perfor...[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-performance liquid chromatography-high resolution quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)was used to establish a fast screening method for 59 non-standard components in five categories of antiviral agents,aminoglycosides,quinolones,sulfonamides,and tetracyclines in veterinary drugs.The target drugs were separated by a Waters ACQUITY UPLC HSS T3 chromatographic column(50 mm×2.1 mm,1.8μm),and data were collected in the positive ion mode.Good separation of the 59 drugs was achieved within 7 min.[Results]In the concentration range of 0-100 ng/ml,each drug showed a good linear relationship,and the correlation coefficients were all greater than 0.999.The detection limits of the 59 drugs were in the range of 0.1-0.5 mg/ml,and the recovery under the addition concentration of 5 mg/ml was in the range of 85.2%-103.8%.[Conclusions]The method is fast,simple,accurate,and highly sensitive,and is suitable for high-throughput screening and qualitative identification of non-standard components in veterinary drug preparations.展开更多
Isolation and comparison of uremic sera and urine and normal sera and urine were performed by gel permeation chromatography, anion exchange chromatography and reversed-phase high performance liquid chromatography. Two...Isolation and comparison of uremic sera and urine and normal sera and urine were performed by gel permeation chromatography, anion exchange chromatography and reversed-phase high performance liquid chromatography. Two uremic middle molecular fractions (A and B) were obtained from uremic sera and urine and normal urine by gel permeation chromatography, but not from normal sera. The anion exchange chromatographic results of fraction A from different origins demonstrate that subfraction A-3 could be excreted in urine by healthy subject, but accumulated in uremic serum for renal failure of patient with uremia. After desalinization subfraction A-3 was analyzed by MALDI-TOF-MS. The results show that subfraction A-3 consists of six compounds with molecular weight 839, 873, 1007.94, 1106, 1680 and 2015 respectively. Finally, by reversed-phase high performance liquid chromatography, subfraction A-3 was further resolved into six independent fractions. Thus, the isolation and purification of six middle molecular compounds in subfraction A-3 came true by our method.展开更多
A detailed stratigraphic investigation of the intercalation mechanism when graphite electrodes are immersed inside diluted perchloric(HClO_(4))and sulfuric(H_(2)SO_(4))electrolytes is obtained by comparing results whe...A detailed stratigraphic investigation of the intercalation mechanism when graphite electrodes are immersed inside diluted perchloric(HClO_(4))and sulfuric(H_(2)SO_(4))electrolytes is obtained by comparing results when graphite crystals are simply immersed in the same acid solutions.By combining time-of-flight secondary ion mass spectrometry(ToF-SIMS)and in-situ atomic force microscopy(AFM),we provide a picture of the chemical species involved in the intercalation reaction.The depth intensity profile of the ion signals along the electrode crystal clearly shows a more complex mechanism for the intercalation process,where the local morphology of the basal plane plays a crucial role.Solvated anions are mostly located within the first tens of nanometers of graphite,but electrolytes also diffuse inside the buried layers for hundreds of nanometers,the latter process is also aided by the presence of mesoscopic crystal defects.Residual material from the electrolyte solution was found localized in well-defined circular spots,which represent preferential interaction areas.Interestingly,blister-like micro-structures similar to those observed on the highly oriented pyrolytic graphite(HOPG)surface were found in the buried layers,confirming the equivalence of the chemical condition on the graphite surface and in the underneath layers.展开更多
基金Supported by Key R&D Projects in Hebei Province(19227516D)Hebei Provincial PhaseⅡModern Agricultural Industry Technology System Innovation Team Building Project(HBCT2018120207,HBCT2018160403)Hebei Province Innovation Ability Promotion Plan Project(20567673H)。
文摘Milk and dairy products are more and more popular with consumers due to their various nutrients, and their quality and safety issues have always been concerned. Therefore, the development of rapid, accurate and simple screening techniques is of great significance. Liquid chromatography-high resolution time-of-flight mass spectrometry has high-resolution and high-throughput detection functions, and has gradually begun to be applied in the detection of milk and dairy products. This paper summarized the application of milk and dairy products in liquid chromatography-high resolution time-of-flight mass spectrometry, laying a foundation for the development of new methods.
基金supported by the National Natural Science Foundation of China(No.30873196)Project of Modernization of Traditional Chinese Medicine of Shanghai(No.09dZ1975100)
文摘An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis of the analysis of the first dimension, retention components of the urine sample were collected into 30 fractions （one fraction per minute）. Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine （Songorine, 14-benzoylneoline, Deoxyaconitine, etc. ） exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the system suggest that the CMC can be applied to in vivo study.
基金Supported by Key R&D Project of Hebei Province(19227516D)Hebei Provincial Phase II Modern Agricultural Industry Technology System Innovation Team Building Project(HBCT2018120207)+2 种基金Hebei Provincial Phase II Modern Agricultural Industry Technology System Grass Industry Innovation Team Building Project(HBCT2018160403)Hebei Provincial Science and Technology Innovation Leading Talents(21130243A)The Fourth Batch of High-end Talent Project in Hebei Province。
文摘[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-performance liquid chromatography-high resolution quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)was used to establish a fast screening method for 59 non-standard components in five categories of antiviral agents,aminoglycosides,quinolones,sulfonamides,and tetracyclines in veterinary drugs.The target drugs were separated by a Waters ACQUITY UPLC HSS T3 chromatographic column(50 mm×2.1 mm,1.8μm),and data were collected in the positive ion mode.Good separation of the 59 drugs was achieved within 7 min.[Results]In the concentration range of 0-100 ng/ml,each drug showed a good linear relationship,and the correlation coefficients were all greater than 0.999.The detection limits of the 59 drugs were in the range of 0.1-0.5 mg/ml,and the recovery under the addition concentration of 5 mg/ml was in the range of 85.2%-103.8%.[Conclusions]The method is fast,simple,accurate,and highly sensitive,and is suitable for high-throughput screening and qualitative identification of non-standard components in veterinary drug preparations.
基金This work was supported by the State Key Fundamental R & D Project (Grant No. G1999064707)the National Natural Science Foundation of China (Grant No. 59873011) Trans-Century Training Program Foundation for the Talents by the Ministry of Education,
文摘Isolation and comparison of uremic sera and urine and normal sera and urine were performed by gel permeation chromatography, anion exchange chromatography and reversed-phase high performance liquid chromatography. Two uremic middle molecular fractions (A and B) were obtained from uremic sera and urine and normal urine by gel permeation chromatography, but not from normal sera. The anion exchange chromatographic results of fraction A from different origins demonstrate that subfraction A-3 could be excreted in urine by healthy subject, but accumulated in uremic serum for renal failure of patient with uremia. After desalinization subfraction A-3 was analyzed by MALDI-TOF-MS. The results show that subfraction A-3 consists of six compounds with molecular weight 839, 873, 1007.94, 1106, 1680 and 2015 respectively. Finally, by reversed-phase high performance liquid chromatography, subfraction A-3 was further resolved into six independent fractions. Thus, the isolation and purification of six middle molecular compounds in subfraction A-3 came true by our method.
基金the European Unions Horizon 2020 research and innovation program under Grant Agreement(No.688225)(Metro4-3D)the National Institute for Nuclear Physics in the framework of the CSN5 Call Project FIRE(Flexible Ionizing Organic Radiation Detectors)LASR3 Surface Analysis Laboratory Roma Tre gratefully acknowledges financial support from uFondazione Roma5(No.5229441F37).
文摘A detailed stratigraphic investigation of the intercalation mechanism when graphite electrodes are immersed inside diluted perchloric(HClO_(4))and sulfuric(H_(2)SO_(4))electrolytes is obtained by comparing results when graphite crystals are simply immersed in the same acid solutions.By combining time-of-flight secondary ion mass spectrometry(ToF-SIMS)and in-situ atomic force microscopy(AFM),we provide a picture of the chemical species involved in the intercalation reaction.The depth intensity profile of the ion signals along the electrode crystal clearly shows a more complex mechanism for the intercalation process,where the local morphology of the basal plane plays a crucial role.Solvated anions are mostly located within the first tens of nanometers of graphite,but electrolytes also diffuse inside the buried layers for hundreds of nanometers,the latter process is also aided by the presence of mesoscopic crystal defects.Residual material from the electrolyte solution was found localized in well-defined circular spots,which represent preferential interaction areas.Interestingly,blister-like micro-structures similar to those observed on the highly oriented pyrolytic graphite(HOPG)surface were found in the buried layers,confirming the equivalence of the chemical condition on the graphite surface and in the underneath layers.
