Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extract...Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extracted from the dog serum using dichlromethane followed by derivatization with DNBF for 20 min at 100℃. The solvent was then evaporated at 60℃ under nitrogen, and the residue was taken up in 100 μL of mobile phase consisting of acetonitrile water (75∶30, v/v). The separation was performed on a Hypersil BDS C18 column with a flow rate of 0 8 mL·min -1 , and the ultraviolet detector wavelength was set at 350 nm. Results Extraction recovery ranged from 75.9% to 83.2%, and methodological recovery was between 96.5% and 109.3%. Within day RSD ranged from 1.5% to 6.3%, and inter day RSD was between 2 9% and 14.8%. The method showed good linearity (R=0.9998). Conclusion The method was simple, convenient and sensitive. The reaction of derivatization was reproducible.展开更多
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
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
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
采用柱前衍生化高效液相色谱法,对罗望子胶中主要单糖组分进行检测。选用Diamonsil-plus C 18-A^(*)色谱柱,用磷酸盐缓冲液-乙腈溶液流动相进行等度洗脱,流速设置1.0 mL/min,柱温35℃,进样量5μL,检测波长245 nm。罗望子胶中主要单糖组...采用柱前衍生化高效液相色谱法,对罗望子胶中主要单糖组分进行检测。选用Diamonsil-plus C 18-A^(*)色谱柱,用磷酸盐缓冲液-乙腈溶液流动相进行等度洗脱,流速设置1.0 mL/min,柱温35℃,进样量5μL,检测波长245 nm。罗望子胶中主要单糖组分葡萄糖、木糖和半乳糖的比例为52.05%、20.03%和12.17%。数据在各自浓度范围内线性关系良好(R≥0.9992),加样回收率在100.33%~101.34%之间,RSD小于2.0%,检测限在0.0005~0.0009 mg/L之间。综上,该检测方法适用于罗望子多糖胶中单糖组分测定。展开更多
文摘Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extracted from the dog serum using dichlromethane followed by derivatization with DNBF for 20 min at 100℃. The solvent was then evaporated at 60℃ under nitrogen, and the residue was taken up in 100 μL of mobile phase consisting of acetonitrile water (75∶30, v/v). The separation was performed on a Hypersil BDS C18 column with a flow rate of 0 8 mL·min -1 , and the ultraviolet detector wavelength was set at 350 nm. Results Extraction recovery ranged from 75.9% to 83.2%, and methodological recovery was between 96.5% and 109.3%. Within day RSD ranged from 1.5% to 6.3%, and inter day RSD was between 2 9% and 14.8%. The method showed good linearity (R=0.9998). Conclusion The method was simple, convenient and sensitive. The reaction of derivatization was reproducible.
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.
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).
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.
