Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new met...Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new method is described for the determination of sparfloxacin in human urine. The linear range is 0.05 mg/L to 4.0 mg/L, the recoveries are 91.5%similar to 95.7% and the RSD is 1.2%similar to4.2%. The results showed that this method is suitable for the determination of sparfloxacin in human urine.展开更多
A rapid and accurate quantitative method of high performance liquid chromatography( HPLC) with fluorescence detector has been developed for the analysis of 18 kinds of amino acids in fresh tea leaves. The samples were...A rapid and accurate quantitative method of high performance liquid chromatography( HPLC) with fluorescence detector has been developed for the analysis of 18 kinds of amino acids in fresh tea leaves. The samples were minced and mixed,and extracted with ultra pure water at 90℃ for 20 min. The 6-aminoquinolyl N-hydroxy-succinimidyl carbamate( AQC) was used as pre-column derivatization reagent. Gradient HPLC separation was performed on a C_(18) column( Symmetry C_(18),3. 9 mm × 15 cm,4 μm). Good linearity between concentrations and peak areas was achieved in the concentration range of 5. 0-250 μmol/L for 18 kinds of amino acids. The method was validated by the analysis of five replicates. The 18 kinds of amino acid standards were spiked in fresh tea leaf samples and the average recovery rate was 86. 25%-109. 05% with relative standard deviations( n = 5) ranging from 6. 03% to 10. 56%. The limit of detection( LOD) for the analytes was0. 05-1. 27 μmol/L. The method was successfully applied to the analysis of the 18 kinds of amino acids in fresh tea leaves from east Dongting and west Dongting mountains in Suzhou. The results indicate that the method is simple,rapid,precise and reliable.展开更多
Bonding fiber reinforced polymer (FRP) has been commonly used to improve the seismic behavior of circular reinforced concrete (RC) columns in engineering practice. However, FRP jackets have a significant stress hy...Bonding fiber reinforced polymer (FRP) has been commonly used to improve the seismic behavior of circular reinforced concrete (RC) columns in engineering practice. However, FRP jackets have a significant stress hysteresis effect in this strengthening method, and pre-tensioning the FRP can overcome this problem. This paper presents test results of 25 circular RC columns strengthened with pre-stressed FRP strips under low cyclic loading. The pre-stressing of the FRP strips, types of FRP strips and longitudinal reinforcement, axial load ratio, pre-damage degree and surface treatments of the specimens are considered as the primary factors in the tests. According to the failure modes and hysteresis curves of the specimens, these factors are analyzed to investigate their effect on bearing capacity, ductility, hysteretic behavior, energy dissipation capacity and other important seismic behaviors. The results show that the initial lateral confined stress provided by pre-stressed FRP strips can effectively inhibit the emergence and development of diagonal shear cracks, and change the failure modes of specimens from brittle shear failure to bending or bending-shear failure with better ductility. As a result, the bearing capacity, ductility, energy dissipation capacity and deformation capacity of the strengthened specimens are all significantly improved.展开更多
High performance liquid chromatography method for the separation of a series of chiral benzyl alcohols on N-(3,5-dinitrobenzoyl)-D-phenylglycine stationary phase (Macherey Nagel, Chiral-2) after pre-column achiral der...High performance liquid chromatography method for the separation of a series of chiral benzyl alcohols on N-(3,5-dinitrobenzoyl)-D-phenylglycine stationary phase (Macherey Nagel, Chiral-2) after pre-column achiral derivatization was developed. Cheap and easy available aromatic acid chlorides were used as derivatization agents. Good to excellent separations of the enantiomers were achieved in all cases in relatively short analytical runs. It was shown that the enantiorecognition depends on the substituents both in the starting alcohol and in the acid chloride. The method presents an efficient alternative to the direct analyses on polysaccharide and cyclodextrine-derived stationary phases.展开更多
A simple, sensitive and precise green high-performance liquid chromatographic method including on-line pre-column oxidation combined by column switching with a short Hypersil ODS analytical column (100 mm × 4.0 m...A simple, sensitive and precise green high-performance liquid chromatographic method including on-line pre-column oxidation combined by column switching with a short Hypersil ODS analytical column (100 mm × 4.0 mm i.d.) for enrichment and separation was developed and validated to determine low levels of methotrexate (MTX). The method was based on oxidative cleavage of MTX into highly fluorescence products, 2,4-diaminopteridine-6-carboxaldehyde and the corresponding 2,4-diaminopteridine-6-carboxylic acid, during the flow of phosphate buffer (0.04 M, pH 3.4) containing the analyte through the packed reactor of cerium (IV) trihydroxyhydroperoxide (CTH) at a flow-rate of 0.2 mL/min and 40℃. The fluorescent products were enriched on the head of ODS analytical column for the final separation. The separation was performed at room temperature using an environmentally friendly mobile phase consisting of ethanol and phosphate buffer (0.04 M, pH 3.4) in the ratio of 10:90 (v/v). The eluent was monitored at emission and excitation wavelengths of 463 and 367 nm, respectively. The method was successfully applied, without any interference from the excipients, for the determination of drug in tablets and vials with a detection limit of 0.06 ng/mL from 500 ?L of sample MTX.展开更多
动脉粥样硬化是心血管疾病重要的病理生理基础,延缓和防治动脉粥样硬化对于减少和降低心血管疾病的发病率及病死率具有重要意义。高密度脂蛋白(high density lipoprotein,HDL)通过参与介导胆固醇逆向转运(reverse cholesterol transport...动脉粥样硬化是心血管疾病重要的病理生理基础,延缓和防治动脉粥样硬化对于减少和降低心血管疾病的发病率及病死率具有重要意义。高密度脂蛋白(high density lipoprotein,HDL)通过参与介导胆固醇逆向转运(reverse cholesterol transport,RCT)在抗动脉粥样硬化的形成和进展中发挥了重要作用。Preβ-1高密度脂蛋白(prebeta-1 high density lipoprotein,Preβ-1HDL)作为HDL的一种亚类,是外周细胞移出胆固醇的最初接受体,直接参与了RCT的起始步骤,并在随后的胆固醇酯化及转运中起着重要作用。本文就Preβ-1HDL的结构、代谢及其与心血管疾病的关系作一简要综述。展开更多
A sensitive high-performance chromatographic method for the detection of N-nitrosoamines with pre-column fluorescence derivatization has been developed.Eight representative N-nitrosoamines, which were separated on a r...A sensitive high-performance chromatographic method for the detection of N-nitrosoamines with pre-column fluorescence derivatization has been developed.Eight representative N-nitrosoamines, which were separated on a reversed-phase C18column with methanol - Water-triethylamine as eluent, were used as model compounds to optimize the derivathation and the chromatographic conditions. The relative standard deviations(n=7) at an analytical concentration of 4×10-6 mol/L are less than 5%. The detection limits (signal-to-noise ratio=3) for the N-nitrosoamines compounds are in the range of 0.02~0. 14 nmol per injection volume(10μl).展开更多
文摘Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new method is described for the determination of sparfloxacin in human urine. The linear range is 0.05 mg/L to 4.0 mg/L, the recoveries are 91.5%similar to 95.7% and the RSD is 1.2%similar to4.2%. The results showed that this method is suitable for the determination of sparfloxacin in human urine.
基金Supported by Open Project of the Key Laboratory of Food Quality and Safety of Jiangsu Province-State Key Laboratory Breeding Base(201603)Basic Research Project of Application of Suzhou City(SNG201622)
文摘A rapid and accurate quantitative method of high performance liquid chromatography( HPLC) with fluorescence detector has been developed for the analysis of 18 kinds of amino acids in fresh tea leaves. The samples were minced and mixed,and extracted with ultra pure water at 90℃ for 20 min. The 6-aminoquinolyl N-hydroxy-succinimidyl carbamate( AQC) was used as pre-column derivatization reagent. Gradient HPLC separation was performed on a C_(18) column( Symmetry C_(18),3. 9 mm × 15 cm,4 μm). Good linearity between concentrations and peak areas was achieved in the concentration range of 5. 0-250 μmol/L for 18 kinds of amino acids. The method was validated by the analysis of five replicates. The 18 kinds of amino acid standards were spiked in fresh tea leaf samples and the average recovery rate was 86. 25%-109. 05% with relative standard deviations( n = 5) ranging from 6. 03% to 10. 56%. The limit of detection( LOD) for the analytes was0. 05-1. 27 μmol/L. The method was successfully applied to the analysis of the 18 kinds of amino acids in fresh tea leaves from east Dongting and west Dongting mountains in Suzhou. The results indicate that the method is simple,rapid,precise and reliable.
基金National Natural Science Foundation of China under Grant No.51178029 State Key Laboratory for Disaster Reduction in Civil Engineering at Tongji University under Grant No.SLDRCE08-MB-01
文摘Bonding fiber reinforced polymer (FRP) has been commonly used to improve the seismic behavior of circular reinforced concrete (RC) columns in engineering practice. However, FRP jackets have a significant stress hysteresis effect in this strengthening method, and pre-tensioning the FRP can overcome this problem. This paper presents test results of 25 circular RC columns strengthened with pre-stressed FRP strips under low cyclic loading. The pre-stressing of the FRP strips, types of FRP strips and longitudinal reinforcement, axial load ratio, pre-damage degree and surface treatments of the specimens are considered as the primary factors in the tests. According to the failure modes and hysteresis curves of the specimens, these factors are analyzed to investigate their effect on bearing capacity, ductility, hysteretic behavior, energy dissipation capacity and other important seismic behaviors. The results show that the initial lateral confined stress provided by pre-stressed FRP strips can effectively inhibit the emergence and development of diagonal shear cracks, and change the failure modes of specimens from brittle shear failure to bending or bending-shear failure with better ductility. As a result, the bearing capacity, ductility, energy dissipation capacity and deformation capacity of the strengthened specimens are all significantly improved.
文摘High performance liquid chromatography method for the separation of a series of chiral benzyl alcohols on N-(3,5-dinitrobenzoyl)-D-phenylglycine stationary phase (Macherey Nagel, Chiral-2) after pre-column achiral derivatization was developed. Cheap and easy available aromatic acid chlorides were used as derivatization agents. Good to excellent separations of the enantiomers were achieved in all cases in relatively short analytical runs. It was shown that the enantiorecognition depends on the substituents both in the starting alcohol and in the acid chloride. The method presents an efficient alternative to the direct analyses on polysaccharide and cyclodextrine-derived stationary phases.
文摘A simple, sensitive and precise green high-performance liquid chromatographic method including on-line pre-column oxidation combined by column switching with a short Hypersil ODS analytical column (100 mm × 4.0 mm i.d.) for enrichment and separation was developed and validated to determine low levels of methotrexate (MTX). The method was based on oxidative cleavage of MTX into highly fluorescence products, 2,4-diaminopteridine-6-carboxaldehyde and the corresponding 2,4-diaminopteridine-6-carboxylic acid, during the flow of phosphate buffer (0.04 M, pH 3.4) containing the analyte through the packed reactor of cerium (IV) trihydroxyhydroperoxide (CTH) at a flow-rate of 0.2 mL/min and 40℃. The fluorescent products were enriched on the head of ODS analytical column for the final separation. The separation was performed at room temperature using an environmentally friendly mobile phase consisting of ethanol and phosphate buffer (0.04 M, pH 3.4) in the ratio of 10:90 (v/v). The eluent was monitored at emission and excitation wavelengths of 463 and 367 nm, respectively. The method was successfully applied, without any interference from the excipients, for the determination of drug in tablets and vials with a detection limit of 0.06 ng/mL from 500 ?L of sample MTX.
文摘动脉粥样硬化是心血管疾病重要的病理生理基础,延缓和防治动脉粥样硬化对于减少和降低心血管疾病的发病率及病死率具有重要意义。高密度脂蛋白(high density lipoprotein,HDL)通过参与介导胆固醇逆向转运(reverse cholesterol transport,RCT)在抗动脉粥样硬化的形成和进展中发挥了重要作用。Preβ-1高密度脂蛋白(prebeta-1 high density lipoprotein,Preβ-1HDL)作为HDL的一种亚类,是外周细胞移出胆固醇的最初接受体,直接参与了RCT的起始步骤,并在随后的胆固醇酯化及转运中起着重要作用。本文就Preβ-1HDL的结构、代谢及其与心血管疾病的关系作一简要综述。
文摘A sensitive high-performance chromatographic method for the detection of N-nitrosoamines with pre-column fluorescence derivatization has been developed.Eight representative N-nitrosoamines, which were separated on a reversed-phase C18column with methanol - Water-triethylamine as eluent, were used as model compounds to optimize the derivathation and the chromatographic conditions. The relative standard deviations(n=7) at an analytical concentration of 4×10-6 mol/L are less than 5%. The detection limits (signal-to-noise ratio=3) for the N-nitrosoamines compounds are in the range of 0.02~0. 14 nmol per injection volume(10μl).