建立了虾中14种磺胺类药物残留量的柱后衍生高效液相色谱检测方法。样品在加入内标物磺胺吡啶后用乙酸乙酯提取，提取液浓缩后用4 mL 乙酸乙酯溶解残余物，用盐酸溶液反萃取，正己烷去脂，盐酸溶液经滤膜过滤后，加入乙腈、甲醇和3.5 mo...建立了虾中14种磺胺类药物残留量的柱后衍生高效液相色谱检测方法。样品在加入内标物磺胺吡啶后用乙酸乙酯提取，提取液浓缩后用4 mL 乙酸乙酯溶解残余物，用盐酸溶液反萃取，正己烷去脂，盐酸溶液经滤膜过滤后，加入乙腈、甲醇和3.5 mol / L 乙酸钠溶液（体积比为5：5：20）的混合溶液混匀后，经高效液相色谱分离，用荧光胺衍生试剂进行柱后衍生，荧光检测器检测。采用基质标样添加法绘制标准曲线，内标法定量。对柱后衍生系统参数进行了优化，确定了荧光胺溶液的浓度、流速和反应温度分别为0.2 g / L、0.15 mL / min 和50℃。14种磺胺类药物在5～200μg / L 范围内具有良好的线性。磺胺类药物的定量限（LOQ，S / N =10）为1.0～5.0μg / kg。在1.0～100.0μg / kg 添加水平内，磺胺类药物的平均回收率为77.8％～103.6％，相对标准偏差（ RSD）为2.9％～9.1％（ n =6）。实验结果表明该方法灵敏、准确，重复性好，适用于虾中磺胺类药物的残留检测。展开更多
A simple, rapid and sensitive high performance liquid chromatography （HPLC） method was developed for the determination of metoclopramide in pharmaceutical preparation. The method is based on the derivatization of me...A simple, rapid and sensitive high performance liquid chromatography （HPLC） method was developed for the determination of metoclopramide in pharmaceutical preparation. The method is based on the derivatization of metoclopramide with fluorescamine. The separation was achieved on a C18 column using methanol-water （70 ： 30, V/V） mobile phase. Fluorescence detector was used at the excitation and emission of 403 and 485 nm, respectively. The method was validated for linearity, limit of detection, limit of quantification, precision, accuracy, recovery, robust- ness and system suitability. The assay was linear over the concentration range of 100-2000 ng/mL. The mean recovery was 100.37%. The proposed method was successfully applied to the assay of metoclopramide in tablet preparation. The preparation was also analyzed with an official method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level.展开更多
Zinc may play a role as a co-factor in the pathogenesis of Alzheimer＇s disease （AD） through influencing the conformation and neurotoxicity of amyloid β-protein （Aβ）. Using the fluorescamine assay, we show for t...Zinc may play a role as a co-factor in the pathogenesis of Alzheimer＇s disease （AD） through influencing the conformation and neurotoxicity of amyloid β-protein （Aβ）. Using the fluorescamine assay, we show for the first time that Zn^2＋ induced Aβ（10-21） aggregate in a concentration-dependent manner. These results indicate that Aβ（10-21） can be used as an in vitro model in Zn^2＋ - induced Aβ aggregation and that the region 10-21 to be the minimal fragment of zinc-binding domain of full length Aβ（1-42）.展开更多
The objective of this study was to improve primary-amine nitrogen (1°-N) quantification in dissolved organic matter (DOM) originating from natural waters where inorganic forms of N, which may cause analytical int...The objective of this study was to improve primary-amine nitrogen (1°-N) quantification in dissolved organic matter (DOM) originating from natural waters where inorganic forms of N, which may cause analytical interference, are commonly encountered. Efforts were targeted at elucidating organic-N structural criteria influencing the response of organic amines to known colorimetric and fluorescent reagents and exploring the use of divalent metal-assisted amide hydrolysis in combination with fluorescence analyse...展开更多
A self-ordered ring(SOR) fluorescence microscopic imaging technique has been developed for the determination of trace amounts of sulfadiazine based on its derivatization with fluorescamine.In the presence of HAc-NaAc ...A self-ordered ring(SOR) fluorescence microscopic imaging technique has been developed for the determination of trace amounts of sulfadiazine based on its derivatization with fluorescamine.In the presence of HAc-NaAc buffer solution(pH 3.12) and polyvinyl alcohol-124(PVA-124),the droplet containing fluorescamine derivatized sulfadiazine can form a SOR on the solid support after solvent evaporation with the diameter of 1.86mm and its ring belt width of 54.9 μ m.The quantitative analysis of sulfadiazine is achieved with the linear range of 7.8×10-14 ～1.8×10-12 mol·ring-1(3.9×10-7 ～9.0×10-6 mol·L-1) and detection limit of 7.8×10-15 mol·ring-1(3.9×10-8 mol·L-1) when 0.2 μ L droplet was spotted.The technique has been satisfactorily applied to the determination of sulfadiazine in the tablet,synthetic sample and residues in six different milk samples with the recoveries of 91.0%～105.8%,respectively,and RSDs less than 4.4%.展开更多
文摘建立了虾中14种磺胺类药物残留量的柱后衍生高效液相色谱检测方法。样品在加入内标物磺胺吡啶后用乙酸乙酯提取，提取液浓缩后用4 mL 乙酸乙酯溶解残余物，用盐酸溶液反萃取，正己烷去脂，盐酸溶液经滤膜过滤后，加入乙腈、甲醇和3.5 mol / L 乙酸钠溶液（体积比为5：5：20）的混合溶液混匀后，经高效液相色谱分离，用荧光胺衍生试剂进行柱后衍生，荧光检测器检测。采用基质标样添加法绘制标准曲线，内标法定量。对柱后衍生系统参数进行了优化，确定了荧光胺溶液的浓度、流速和反应温度分别为0.2 g / L、0.15 mL / min 和50℃。14种磺胺类药物在5～200μg / L 范围内具有良好的线性。磺胺类药物的定量限（LOQ，S / N =10）为1.0～5.0μg / kg。在1.0～100.0μg / kg 添加水平内，磺胺类药物的平均回收率为77.8％～103.6％，相对标准偏差（ RSD）为2.9％～9.1％（ n =6）。实验结果表明该方法灵敏、准确，重复性好，适用于虾中磺胺类药物的残留检测。
文摘A simple, rapid and sensitive high performance liquid chromatography （HPLC） method was developed for the determination of metoclopramide in pharmaceutical preparation. The method is based on the derivatization of metoclopramide with fluorescamine. The separation was achieved on a C18 column using methanol-water （70 ： 30, V/V） mobile phase. Fluorescence detector was used at the excitation and emission of 403 and 485 nm, respectively. The method was validated for linearity, limit of detection, limit of quantification, precision, accuracy, recovery, robust- ness and system suitability. The assay was linear over the concentration range of 100-2000 ng/mL. The mean recovery was 100.37%. The proposed method was successfully applied to the assay of metoclopramide in tablet preparation. The preparation was also analyzed with an official method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level.
基金This work was supported by the National Natural Science Foundation of China(No.30470408).
文摘Zinc may play a role as a co-factor in the pathogenesis of Alzheimer＇s disease （AD） through influencing the conformation and neurotoxicity of amyloid β-protein （Aβ）. Using the fluorescamine assay, we show for the first time that Zn^2＋ induced Aβ（10-21） aggregate in a concentration-dependent manner. These results indicate that Aβ（10-21） can be used as an in vitro model in Zn^2＋ - induced Aβ aggregation and that the region 10-21 to be the minimal fragment of zinc-binding domain of full length Aβ（1-42）.
基金the Andrew Mellon Foundation,NSF Biocomplexity Program (Richter)NSF Career Grant BES-9984489(Vasudevan)and the EPA-STAR program (Fimmen) for funding.
文摘The objective of this study was to improve primary-amine nitrogen (1°-N) quantification in dissolved organic matter (DOM) originating from natural waters where inorganic forms of N, which may cause analytical interference, are commonly encountered. Efforts were targeted at elucidating organic-N structural criteria influencing the response of organic amines to known colorimetric and fluorescent reagents and exploring the use of divalent metal-assisted amide hydrolysis in combination with fluorescence analyse...
基金The National Nature Science Foundation of China(Grant Nos.20767004,21177163)111 Project B08044+1 种基金"985 Project"of Minzu University of China(MUC 98507-08)"211 Project"of Minzu University of China(MUC 02121103)
文摘A self-ordered ring(SOR) fluorescence microscopic imaging technique has been developed for the determination of trace amounts of sulfadiazine based on its derivatization with fluorescamine.In the presence of HAc-NaAc buffer solution(pH 3.12) and polyvinyl alcohol-124(PVA-124),the droplet containing fluorescamine derivatized sulfadiazine can form a SOR on the solid support after solvent evaporation with the diameter of 1.86mm and its ring belt width of 54.9 μ m.The quantitative analysis of sulfadiazine is achieved with the linear range of 7.8×10-14 ～1.8×10-12 mol·ring-1(3.9×10-7 ～9.0×10-6 mol·L-1) and detection limit of 7.8×10-15 mol·ring-1(3.9×10-8 mol·L-1) when 0.2 μ L droplet was spotted.The technique has been satisfactorily applied to the determination of sulfadiazine in the tablet,synthetic sample and residues in six different milk samples with the recoveries of 91.0%～105.8%,respectively,and RSDs less than 4.4%.
