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1.
液相色谱/蒸发光散射测定转基因烟草提取液中的海藻糖 总被引:6,自引:0,他引:6
采用乙二胺动态修饰硅胶柱分离、蒸发光散射检测器测定了转基因烟草提取液中的糖。 4种糖的峰面积标准曲线在 10 0mg/L~ 15 0 0mg/L范围内均具有良好的线性关系。所建立的方法对果糖、葡萄糖、蔗糖、海藻糖的检测下限分别为 10mg/L ,2 0mg/L ,10mg/L和 10mg/L。 相似文献
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纤维素三(3,5-二甲基苯基氨基甲酸酯)是液相色谱中使用最广泛的手性柱。该文详细地研究了不同程度衍生的纤维素(3,5-二甲基苯基氨基甲酸酯)以及不同硅胶(粗制硅胶、氨丙基粗制硅胶、精制硅胶、氨丙基精制硅胶、大孔硅胶、氨丙基大孔硅胶)作为支撑体对该柱手性分离能力的影响。自制了13根手性色谱柱,分别考察了其对16种外消旋体的拆分,分离结果显示:三取代纤维素柱 > 二取代纤维素柱 > 纤维素柱;精制硅胶和大孔硅胶优于粗制硅胶,大孔硅胶的柱压更低;硅胶的氨丙基化对手性选择性有一定的影响;这些手性柱之间具有一定的互补性,尤其是纤维素柱。该文有助于人们更深刻地理解和更好地把握高效液相色谱手性柱的制备。 相似文献
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研究了非晶硅膜改性的弹性玻璃毛细管交联OV-1701中等极性固定相色谱柱。在适当温度下,采用过氧化二异丙苯(DCUP)游离基引发交联OV-1701固定液,成功地制备了交联OV-1701柱,该柱具有柱效高、惰性好、耐溶剂、抗腐蚀和耐高温等性能,是一种新型高性能的中等极性交联柱。 相似文献
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高效液相色谱法分析蜂蜜中的糖 总被引:9,自引:4,他引:9
本文研究了用四乙撑五胺(简称TEPA)作为胺基改善剂,在硅胶柱上定量分析蜂蜜含糖量的方法,并成功地分离了木糖、果糖、葡萄糖、蔗糖、麦芽糖和乳糖。对操作条件进行了探讨。采用示差折光检测器检测,含0.01%TEPA的乙腈-水(77+23)作流动相。六种糖的相对标准偏差均小于3.5%。 相似文献
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Superox系列固定相是性能优良的氢键型固定相,适用地脂肪醇分析,非级性固定相OV-1柱,经减活处理后亦适宜醇类异构体分离,考察了C1-C2异构醇的36个组分在分离效能。OV-1柱和Superox0.6柱上的保留行为,柱效和极限温度,结果表明,两种柱对醇都有很好的分离效能。OV-1柱柱效及柱温极限高,除了戊醇-3和戊醇-2是重叠峰外,其余组分间有一定分离度,其分离顺序基本上是根据组分的沸点,包括 相似文献
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黄酮类化合物的超临界流体色谱分离 总被引:18,自引:0,他引:18
利用超临界流体色谱成功地分离了黄酮类化合物,研究了流动相组成,柱条件,压力及温度的影响。发现流动相组成是影响色谱分离的最主要因素;其次,色谱柱条件也是影响分离的一个很重要的因素,硅胶基质的键合苯基柱比较适合于极性黄酮类化合物的分离。 相似文献
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溶胶-凝胶法制备毛细管硅胶整体柱的研究进展 总被引:3,自引:0,他引:3
毛细管硅胶整体柱作为一种新型的分离介质,在色谱领域显示出了强大的生命力。本评述介绍了溶胶-凝胶法制备毛细管硅胶整体柱的方法,重点分析了溶胶-凝胶法制备毛细管硅胶整体柱的影响因素,总结了近几年毛细管硅胶整体柱在高效液相色谱和电色谱中的应用。 相似文献
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液相色谱-串联质谱法同时检测饲料中7种精神类药物 总被引:1,自引:0,他引:1
建立了液相色谱-串联质谱同时检测饲料样品中7种精神类药物(硝西泮、奥沙西泮、氯丙嗪、异丙嗪、地西泮、奋乃静、硫利达嗪)的方法.通过对提取溶剂、净化等预处理条件及LC-MS/MS 分析条件的优化,可以同时检测饲料中7种违禁精神类药物.饲料样品经乙腈/水(9:1, V/V)提取后,过MCX固相萃取柱净化,氮吹至干,用1 mL乙腈/水(2:8, V/V)溶解后测定,采用SRM模式进行定性与定量分析.7种精神类药物在饲料中的回收率为53.9%~110.2%; 相对标准偏差为3.4%~18.4%;硝西泮、奥沙西泮、氯丙嗪、异丙嗪的检出限为1.0 ng/g;对地西泮、奋乃静、硫利达嗪的检出限为5.0 ng/g.结果表明,本方法可用于饲料中7种精神类药物的测定. 相似文献
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A rapid, simple, and sensitive kinetic method is developed for the determination of trace amounts of Sb(V). The method is
based on the reaction of Sb(V) with iodide in acidic media in the presence of methylene blue. The reaction was monitored spectrophotometrically
by measuring the decrease in the absorbance at 664 nm by a fixed-time technique of 60 s. The method allowed the determination
of Sb(V) at concentrations between 0.01 and 2.2 μg/mL. The limit of detection was 0.006 μg/mL and the relative standard deviation
for ten replicate measurements of 0.5 μg/mL Sb(V) was 1.2%. The method was applied to the determination of Sb(V) in tap water
and spring water with satisfactory results.
The text was submitted by the authors in English. 相似文献
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Akiharu Hioki 《Analytical sciences》2008,24(9):1099-1103
A coulometric analysis method and an ion-exclusion chromatographic method were developed for the determination of antimony(V) in a large excess of antimony(III). Antimony(V) reacted with potassium iodide in a high concentration hydrochloric acid; the liberated iodine was determined by the standard-addition method using coulometrically generated iodine. Using a Dionex ICE-AS1 ion-exclusion column, antimony(V) was eluted with 40 mmol/L sulfuric acid; on the other hand, antimony(III) was strongly retained on the column. The content, expressed as the amount ratio of antimony(V) to antimony(III), was 0.035% in a 10 g/kg antimony(III) solution prepared from an antimony(III) oxide reagent by the coulometric analysis method and 0.036% in a 1 g/kg antimony(III) solution prepared from the same antimony(III) oxide by the ion-exclusion chromatographic method. The results of both methods were in good agreement with each other. The detection limit of antimony(V) in antimony(III) oxide by the former method was 0.004% of antimony(III), and that by the latter method was 0.002% of antimony(III). 相似文献
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纤维素-三(3,5-二甲基苯基氨基甲酸酯)涂敷手性固定相的制备、表征及评价 总被引:3,自引:0,他引:3
以纤维素和 3,5 二甲基苯基异氰酸酯为原料合成了纤维素 三 (3,5 二甲基苯基氨基甲酸酯 ) ,并采用两种不同的方法将其涂敷于小粒径 (平均粒径 5 μm ,平均孔径 13nm ,比表面积 110m2 / g)的氨基丙烷化硅胶 (APS)上 ,制得了在纤维素 三 (苯基氨基甲酸酯 )类衍生物涂敷的硅基手性固定相中具有较佳手性识别能力的固定相。通过元素分析、扫描电子显微镜对两种手性固定相进行了表征 ,用高效液相色谱法对两种固定相的手性拆分能力进行了评价和比较。 相似文献
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Fe(Ⅱ)和Ti(Ⅲ)与鲁米诺的化学发光反应已有报道,我们发现,Cr(Ⅱ)、Mo(Ⅲ)、W(Ⅲ)、U(Ⅲ)、CN-、SO32-、抗坏血酸等一大类还原剂均可与鲁米诺溶液作用产生化学发光,本文利用Jones还原柱产生V(Ⅱ),首次研究了V(Ⅱ)与鲁米诺的化学发光反应,在此基础上建立了钒的流动注射化学发光分析法,方法的检出限是8×10-11g/mL钒,线性范围是4×10-10~1×10-5g/mL钒。测定的相对标准偏差小于2%,考察了20余种常见离子对测定的干扰情况,方法已用于水样中痕量钒的测定,初步探讨了发光反应的机理。 相似文献
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Izumi Y Kiyotaki F Yagi N Vlaicu AM Nisawa A Fukushima S Yoshitake H Iwasawa Y 《The journal of physical chemistry. B》2005,109(31):14884-14891
X-ray absorption fine structure combined with X-ray fluorescence spectrometry was applied to various V+TiO2 hybrid samples. Emitted V K alpha1 fluorescence from the sample was selectively counted by using a high-energy-resolution (0.4 eV) spectrometer equipped with a Ge(331) crystal. Two advantages of this method, extremely high signal/background ratio and the compatibility of measurements in the atmosphere of reaction gas (in situ study in relation to heterogeneous catalysis), were effective at the V K-edge. Structure transformation of the V sites was spectroscopically followed for the V/TiO2 catalyst. The monooxo tetrahedral vanadate site was demonstrated to exist at 473 K. It transformed into dispersed species of 5-fold coordination in ambient air and further into polymeric VO(x) species in 0.85 kPa of water at 290 K. In the presence of 3.2 kPa of 2-propanol, dissociative adsorption of 2-propanol on the dispersed V species was strongly suggested at 290-473 K. In situ structure changes of V sites on TiO2 were reported by means of XAFS for the first time. The V(V) sites for the V/TiO2 catalysts were essentially identical with those for V supported on mesoporous (high-surface-area) TiO2 and V-TiO2 sample prepared by the sol-gel method. However, predominant V(IV) sites were found for mesoporous V-TiO2. The V(IV) sites substituted on the Ti sites of TiO2. When the molar ratio of V/Ti increased from 1/100 to 1/5.0, major octahedral V sites in the TiO2 matrix looked to transform into tetrahedral ones. 相似文献
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A simple procedure for selective sorption of tungsten is described. The method involves reduction of W(VI) to W(V) with tin(II) chloride (2%, w/v) at 8-9M hydrochloric acid, formation of the W(V)-SCN complex with 0.2M KSCN and its sorption on polyurethane foam within 20 min. The sorbed complex is then eluted with acidified acetone (1 ml of 1M hydrochloric acid and 8 ml of acetone) followed by addition of 1 ml of 0.1M KSCN to the eluent. The method has been applied to the spectrophotometric determination of tungsten in steels and silicates by measuring the absorbance of the eluted solution at 400 nm. Beer's law is obeyed for the range 0.1-12 mug W/ml. Other elements, e.g., Co(III) (50 mug/ml), Cu(II) (10 mug/ml), Ti(IV) (20 mug/ml), V(V) (10 mug/ml) and Mo(VI) (0.5 mug/ml) have no effect on the method. Interference of copper, up to 100 mug/ml has been eliminated by masking with thiourea and that due to molybdenum by prior separation with thioglycollic acid on PUF. The method has been verified with standard samples. 相似文献
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以聚乙烯吡咯烷酮(PVP)为高分子模板剂,乙酰丙酮钒(C_(15)H_(21)O_6V)和三水合硝酸铜[Cu(NO_3)_2·3H_2O]为原料,导电玻璃(FTO)为载体,结合溶胶-凝胶法和静电纺丝技术制备了前驱体纤维,经高温焙烧后得到分布均匀、具有纤维结构的导电玻璃负载的CuO/V_2O_5复合光电极(CuO/V_2O_5/FTO).采用热重-差热分析仪(TG-DTA)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线光电子能谱仪(XPS)等对材料的结构进行表征,以亚甲基蓝(MB)为目标降解物,探讨了合成产物的光电催化性能.结果表明,CuO与V_2O_5能有效形成异质结构,其光电催化活性均比纯V_2O_5有明显提高,并且改变CuO与V_2O_5的比例对光电催化性能有较大影响,其中n(Cu)∶n(V)=1∶1时降解效率最高,达到96%. 相似文献
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Isha A Yusof NA Ahmad M Suhendra D Yunus WM Zainal Z 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2007,67(5):1398-1402
Fatty hydroxamic acid (FHA) immobilized in polyvinyl chloride (PVC) has been studied as a sensor element of an optical fibre chemical sensor for V(V). By using this instrument, V(V) in solution has been determined in the log concentration range of 0-2.5 (i.e. 1.0-300 mg/L). The detection limit was 1.0 mg/L. The relative standard deviation (R.S.D.) of the method for the reproducibility study at V(V) concentration of 200 mg/L and 300 mg/L were calculated to be 2.9% and 2.0%, respectively. Interference from foreign ions was also studied at 1:1 mole ratio of V(V):foreign ions. It was found that, Fe(III) ion interfered most in the determination of vanadium(V). Excellent agreement with ICP-AES method was achieved when the proposed method was applied towards determination of V(V). 相似文献