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
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 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
建立同时测定水产品中多种生物胺的丹磺酰氯柱前衍生反相高效液相色谱方法。用5％TCA提取样品中生物胺，正己烷脱脂，正丁醇／氯仿（1／1，v／v）萃取，以1，7二胺庚烷为内标，丹磺酰氯为衍生剂衍生后，采用CAPCELL PAK C18MG（4．6mm I...建立同时测定水产品中多种生物胺的丹磺酰氯柱前衍生反相高效液相色谱方法。用5％TCA提取样品中生物胺，正己烷脱脂，正丁醇／氯仿（1／1，v／v）萃取，以1，7二胺庚烷为内标，丹磺酰氯为衍生剂衍生后，采用CAPCELL PAK C18MG（4．6mm I．D．×150mm，5μm）色谱柱，以甲醇／水为流动相，进行梯度洗脱，流速1．5mL／min。荧光检测器的激发波长（Ex）350胁，发射波长（Em）520胁。结果显示：色胺、苯乙胺、腐胺、尸胺、组胺、酪胺、精胺和亚精胺等8种生物胺在30min内完全分离。在给定的浓度范围内，待测生物胺峰面积与内标峰面积之比同其相应浓度呈良好的线性相关（r〉0．99）。仪器重复性良好（RSD〈1．34％），方法重复性也在可接收范围内（RSD〈10％）。除色胺（57．7％）外，其它7种生物胺的样品平均回收率均在94.2％～110．3％之间。结果表明生物胺的HPLC检测方法，分离度好，灵敏度高，可快捷、准确地对水产品中生物胺进行定性和定量检测。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.
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 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).
文摘建立同时测定水产品中多种生物胺的丹磺酰氯柱前衍生反相高效液相色谱方法。用5％TCA提取样品中生物胺，正己烷脱脂，正丁醇／氯仿（1／1，v／v）萃取，以1，7二胺庚烷为内标，丹磺酰氯为衍生剂衍生后，采用CAPCELL PAK C18MG（4．6mm I．D．×150mm，5μm）色谱柱，以甲醇／水为流动相，进行梯度洗脱，流速1．5mL／min。荧光检测器的激发波长（Ex）350胁，发射波长（Em）520胁。结果显示：色胺、苯乙胺、腐胺、尸胺、组胺、酪胺、精胺和亚精胺等8种生物胺在30min内完全分离。在给定的浓度范围内，待测生物胺峰面积与内标峰面积之比同其相应浓度呈良好的线性相关（r〉0．99）。仪器重复性良好（RSD〈1．34％），方法重复性也在可接收范围内（RSD〈10％）。除色胺（57．7％）外，其它7种生物胺的样品平均回收率均在94.2％～110．3％之间。结果表明生物胺的HPLC检测方法，分离度好，灵敏度高，可快捷、准确地对水产品中生物胺进行定性和定量检测。
