钒（Ⅳ）—硫胺素荧光光度法的研究与应用

利用钒（Ⅳ）作为氧化剂将硫胺素氧化成硫胺荧,建立了一种测量痕量硫胺素的荧光分光光度法,并将该方法应用于药物中硫胺素的测定。该方法测定硫胺素的线性范围为０．８～２４０．０μｇ／Ｌ;检出限为０．４５μｇ／Ｌ;对于４０．０μｇ／Ｌ的硫胺素测定１０次,其相对标准偏差为１．５％。     

钒(Ⅴ)-硫胺素荧光反应的研究及应用

本文首次提出了以硫胺素为荧光剂测定微量钒的新方法。该法基于 V(V)-硫胺素反应生成荧光物质,其λ_(ex)=400nm,λ_(em)=464nm,当钒的浓度在2.5×10~(-7)～1.75×10~(-5)mol/L 范围内与荧光强度呈良好的线性关系,用本法测定了粮食样品中的微量钒,获得了满意结果。     

改进的磷钨酸光度法测定水溶液中的钒(Ⅳ)和总钒EI北大核心CSCD

应用改进的磷钨酸光度法测定了样品中总钒和钒(Ⅳ)。在10%HCl介质中,一定体积的待测溶液中添加10%(V:V)H_3PO_4和20%(V:V)的Na_2WO_4·2H_2O(50 g/L)溶液,于30℃下显色30 min。方法的线性范围是0~30 mg/L,线性相关系数R^2=0.9992,相对标准偏差(n=12)为1.2%。并确定了天然水溶液中常见离子干扰钒测定的最大允许量。在此基础上,调节溶液的pH>4,测定V(Ⅳ)。改进后方法测V(Ⅳ)的线性范围为0~5 mg/L,相关系数R^2=0.9998。应用测定自来水和河水中V(Ⅳ)。     

溴酸钾-二甲酚橙体系-顺序注射-催化光度法测定痕量钒

在酸性介质条件下,钒(Ⅳ)能显著催化溴酸钾对二甲酚橙的氧化褪色反应。据此建立了测定痕量钒(Ⅳ)的顺序注射催化光度法。方法的线性范围为0.5~50ng/mL、检出限为0.4ng/mL。对10ng/mL的钒(Ⅳ)连续11次测定的相对标准偏差为1.1%。用于环境水样中痕量钒(Ⅳ)的测定,加标回收率为91%~108%。     

硫胺素-亚硝酸根体系的荧光性质研究及应用

研究了在碱性溶液中硫胺素（VB1）与亚硝酸根的荧光反应,建立了荧光光度法测定硫胺素的新方法。方法线性范围为1．28－324ng/mL,检出限0．52ng/mL,对15个浓度为100ng/mL的硫胺素溶液进行测定,相对标准偏差为1．4％。应用于药物中硫胺素的测定,回收率在96．5％－101．8％之间。     

槲皮素-锡(Ⅳ) 荧光光度法的研究及其应用

研究了槲皮素－锡（Ⅳ）荧光体系的形成条件,建立了测定了槲皮素的荧光度法。在０．００８ｍｏｌ／ＬＨＣｌ介质中,形成ｎ（槲皮素）：ｎ「锡（Ⅳ）」＝２：１的荧光络合物。ＴｒｉｔｏｎＸ－１００对体系有强烈的增敏作用,激发波长为４４３ｎｍ。发射波长为４９５ｎｍ。     

铬—硫胺素荧光光度法测定铬

荧光法测定铬已有报道,但以氧化还原荧光反应为基础的测定方法尚未见报道。木文研究了铬(Ⅳ)-硫胺素(VB_1)体系,发现在3.5—4.0mol/L的硫酸介质中,铬(Ⅵ)-硫胺素反应生成荧光物质硫胺荧:硫胺素 Cr_2O_7~(2-)?硫胺荧 2Cr~(3 )。硫胺荧的激发波长和发射波长分别为λ_(ex)=405mm,λ_(em)=465nm。可以用来作为Cr(Ⅵ)的荧光定量分析。一般荧光法测定铬的方法虽灵敏度较高,但需有机试剂萃取,手续麻烦。本方法则可直接在水相中进行。     

溴酸钾二甲酚橙体系-顺序注射-催化光度法测定痕量钒

在酸性介质条件下,钒(Ⅳ)能显著催化溴酸钾对二甲酚橙的氧化褪色反应。据此建立了测定痕量钒(Ⅳ)的顺序注射催化光度法。方法的线性范围为0.5⁵0ng/mL、检出限为0.4ng/mL。对10ng/mL的钒(Ⅳ)连续11次测定的相对标准偏差为1.1%。用于环境水样中痕量钒(Ⅳ)的测定,加标回收率为91%50ng/mL、检出限为0.4ng/mL。对10ng/mL的钒(Ⅳ)连续11次测定的相对标准偏差为1.1%。用于环境水样中痕量钒(Ⅳ)的测定,加标回收率为91%¹08%。     

Flow-Injection Fluorimetric Determination of Thiamine in Pharmaceutical Preparations

 A new fluorimetric procedure for the determination of thiamine using flow injection analysis is proposed. The method is based on the derivatization reaction of the primary amine group with o-phthalaldehyde in the presence of 2-mercaptoethanol using fluorimetric detection. The calibration graph based on peak area was linear in the range 0.2–6 ng mL⁻¹. The detection limit was close to 0.1 ng mL⁻¹. The method was applied to the determination of the vitamin in commercial pharmaceutical preparations. Received March 31, 1999. Revision October 15, 1999.     

硫胺素—钒（V）—Triton X—100荧光光度法的研究及应用

本文研究了在Trton X-100存在下,琉胺素和钒(Ⅴ)的荧光反应,建立了测定硫胺素的新方法。测定琉胺素的线性范围为2.5×10~(-7)～2.5×10~(-5)mol/L,可用于直接测定生物样品中的硫胺素。     

Fluorimetric Determination of Thiamine with Cobalt(II)

Abstract

A rapid fluorimetric method is reported for the determination of thiamine based upon its interaction with Co(II) ion in the presence of base and a nonionic Triton X-100 micellar medium. The effect of different experimental variables upon the fluorescence intensity were assessed. The detection limit for thiamine is 5.0 × 10^?8M (λ_ex =375nm, λ_em =433nm). The method was successfully applied for determination of thiamine in variety of samples with good accuracy being achieved.     

Fluorimetric Determination of Europium Based on the Co-Fluorescence System Eu-Y-Sparfloxacin-SDS

A new room temperature fluorescence enhancement system based on complex formation between europium and sparfloxacin in the presence of yttrium in sodium dodecyl sulfate micelle solution has been discovered. The characteristic fluorescence spectra and the effect factors of the fluorescence intensity of the system have been studied in detail. The study results show that the binary complex formed by europium with sparfloxacin in sodium dodecyl sulfate micelle solution can emit intrinsic fluorescence of the lanthanide ion. In the presence of yttrium, the fluorescence intensity of this system was enhanced about 5-fold compared with that of the system without Y³⁺. Under the optimum conditions selected, the fluorescence intensity is a linear function of the concentration of europium in the range of 5.0×10^–11–5.0×10^–7molL^–1, and the detection limit of europium is 1.0×10^–13molL^–1. The system was used for the determination of trace amounts of europium in rare earth samples with satisfactory results.     

硫酸颜色反应用于荧光法测定利血平研究

提出了硫酸颜色反应用于利血平的荧光分析新方法。利用血平与浓硫酸反应，生成强荧光物质，所得产物的荧光强度与利血平的浓度在０－０．６μｇ／ｍＬ范围内有良好的线性关系。检测限为０．２ｎｇ／ｍＬ。本法可直接用于尿液中利血平的定量分析，回收率为８２．５％－８４．２％。     

杂多核配位荧光增敏法测定痕量铍

研究了新荧光试剂２－「５－羧基－２－胂酸基苯偶氮」－１,８－二羟基－３,６－萘二碘酸与铍络合的荧光性能。铍与试剂形成荧光络全物,在硼砂介质啼生增敏效应,据此建立了测定痕量铍的新方法。Ｂｅ（Ⅱ）浓度在０－０．１２ｍｇ／Ｌ范围内一荧光哟度呈良好线性关系,方法检测限为０．０７６μｇ／ＬＢｅ（Ⅱ）,用于水及铜基合金样中的痕量铍的测定,结果满意。     

基于固定化酶的流动荧光法测定血清中的葡萄糖

本文将固定化酶柱，光纤以及停流技术结合起来，研究了以廉价而易得的硫胺素为荧光底物的葡萄糖的荧光分析，提出了一种快速、简便、精确地测定葡萄糖的新方法。其线性范围为１．０￣６０．０ｍｇ／Ｌ，线性相关系数为０．９９９，检测限为０．１５ｍｇ／Ｌ。以５．０ｍｇ／Ｌ的葡萄糖作精度试验，ＲＳＤ％＝２．１％（ｎ＝１１）。该方法已成功地用于血清中葡萄糖的测定，结果与光度法相符。     

停流—荧光反应速率仪及其应用于测定维生素B1

本文利用国产930型荧光光度计作为检测器,采用自已制作的流通池,配以蠕动泵及记录仪,组装成停流-荧光动力学分析装置,并用以进行了停流荧光反应速率法测定维生素B_1的研究,利用Hg~(2+)离子在碱性介质中将硫胺素(维生素B_1)氧化为硫胺荧的动力学反应,测定了维生素B_1片剂中维生素B_1的含量。结果表明,这套仪器用于动力学分析,操作简便、省时,维生素B_1的测定结果与标准值基本相符,相对标准偏差为1.28％,其准确度和重现性均令人满意。     

Performance of the Continuous Addition of Reagent Technique in Fluorimetric Reaction-Rate Methods. Determination of Thiamine at the Nanomolar Level

Abstract

The potential of the continuous addition of reagent (CAR) technique, developed for reactions on the millisecond time scale, in fluorimetric reaction-rate methods, is evaluated. The approach was applied to the classical fast reaction involving the oxidation of thiamine to fluorescent thiochrome effected by potassium ferricyanide in basic solutions. Practical problems associated with this system were readily avoided by using the CAR technique. Several kinetic methods have been developed for the determination of thiamine; all are very sentitive (detection limit, 2. 5x10^?9 M) compared to other fluorimetric equilibrium and reaction-rate methods and are suitable for routine analyses (sample throughput, 100 h^?1).     

Derivatization Reaction of Carbohydrates with Urea as the Reagent and Fluorimetric Determination of Carbohydrates

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