吖啶橙催化荧光法测定痕量钒

研究了在酸性介质中柠檬酸存在下,痕量钒（Ｖ）催化溴酸钾氧化吖啶橙退色及其动力学条件,建立了催化荧光法测定痕量钒（Ｖ）的新方法。钒（Ｖ）的线性范围为 ０．２～２．８ μｇ／Ｌ,检出限为 ５．８× １０－８ｇ／Ｌ。３０多种离子基本不干扰测定,将方法用于矿泉水,枸杞和人发样品中钒（Ｖ）的含量的测定,结果满意。此外,还对反应机理进行了初步探讨。     

动力学荧光法测定抗坏血酸

基于在pH 10.7的NH3-NH4Cl缓冲溶液中,抗坏血酸能活化氯化血红素酶催化H2O2氧化L-酪氨酸的反应,使其反应速率增大,将时间驱动技术和动力学中斜率法相结合,建立了一种新的测定抗坏血酸的动力学荧光分析方法。在最佳实验条件下,方法的线性范围为0.1~4.8μg/mL,相对标准偏差3.8%,检出限为1.48μg/L。并考察了环境介质和常见物质的干扰情况。方法可用于实际样品的测定。     

催化动力学荧光法测定痕量甲醛

在硫酸介质中,甲醛能催化溴酸钾氧化藏红T的反应,使其荧光猝灭,据此建立了催化动力学荧光分析法测定甲醛的新方法。研究了催化反应的性能,优化了方法的实验条件。方法的线性范围为0.025~0.25μg/mL,检出限4.19×10-5μg/mL。该方法简便快速,常见共存物质干扰小,已用于环境水样及家居空气中痕量甲醛的测定,结果满意。     

氧化藏红T褪色催化荧光法测定痕量钒

研究了在酸性介质中柠檬酸存在下，痕量钒（Ｖ）催化溴酸钾氧化藏红Ｔ的褪色反应及其动力学条件，建立了催化荧光测定痕量钒的新方法。催化反应在沸水浴中进行８ｍｉｎ，为假零级反应，反应的表观活化能力为９９．２１ｋＪ／ｍｏｌ，反应速度常数为０．１２／ｓ；该方法的检出限为２．２×１０＾－８ｇ／Ｌ；线性范围为０．２￣２．４μｇ／Ｌ研究了共存离子的影响，用于人发和煤灰中痕量钒的测定，结果令人满意。     

钒(Ⅴ)-三溴偶氮胂-溴酸钾催化动力学光度法测定钒

1 引言 钒是人体不可缺少的微量元素之一.适量的钒有利于身体健康,但含量过低或过高都会引起某些器官的病变而出现不适的症状,因而对其准确的测定具有重要的意义.近年来,用催化光度法测定钒引起了人们的广泛兴趣.     

抗坏血酸的催化动力学光度法测定

建立了一种测定抗坏血酸的方便、快速、高灵敏度的催化动力学光度法。对氨基苯磺酸与亚硝酸根进行重氮化反应生成重氮盐,抗坏血酸对重氮盐的分解有催化作用。利用加入8－羟基喹啉与该重氮盐反应生成偶氮染料来终止反应。在波长495nm处,用1cm比色皿以水作参比测定其吸光度,最佳测定酸度为pH9.0。吸光度与空白体系的差值△A与抗坏血酸的质量浓度呈线性关系。该法测定抗坏血酸的线性范围为0．16－6．3mg/L,检出限为0.005mg/L。利用该法测定了维生素C片剂及荔枝晶中的抗坏血酸含量,并与碘量法进行对照,结果基本吻合。     

催化荧光法测定痕量硒

基于稀硝酸介质中溴酸钾氧化藏红T,使其荧光猝灭,硒(Ⅳ)对此反应具有阻抑作用,使荧光强度增大,建立了催化荧光法测定痕量硒(Ⅳ)的新方法。方法检出限为0.12μg L,线性范围为0.5～10μg L。方法可用于测定水样中的硒(Ⅳ)。     

催化荧光法测定人发中痕量钒

钒是人体必须微量元素之一,适量的钒有助于人体健康,由于人体中钒含量极微,选择快速灵敏、选择性好的测定方法,很有必要。催化荧光动力学分析法具有灵敏度高、选择性好的显著特点,近年来用于测钒的报道不少。作者发现,在稀硫酸介质中,以柠檬酸为活化剂,痕量钒（Ⅴ）对溴酸钾氧化二氯荧光素的反应具有很强的催化作用,能使二氯荧光素的荧光强度减小。本文主要研究了该反应的动力学条件,共存离子的影响及人发样中痕量钒的测定,建立了催化荧光法测定痕量钒的方法。     

Fluorimetric kinetic method for the determination of total ascorbic acid with o-phenylenediamine

A fluorimetric reaction-rate method for the determination of L-ascorbic acid (AA) in aqueous solution is presented. The technique is based on the rapid oxidation of AA by mercury(II) chloride to dehydro-L-ascorbic acid, which then reacts with o-phenylenediamine to form a fluorescent quinoxaline. The formation of the product is monitored fluorimetrically with a data acquisition system based on a microcomputer, a voltage-to-frequency converter and a timer-counter board. The initial rate is estimated with a fixed-time computational method. With a 20-s measurement time (after a 5-s delay from initiation of the reaction), the detection limit for AA is 0.02 μg ml^?1 with a linear dynamic range extending to 10 μg ml^?. The procedure is applied to the determination of the AA in vitamin pills and juice. The relative standard deviation is 1.9% or better.     

阻抑动力学荧光法测定柠檬酸

基于在高氯酸介质中柠檬酸能抑制铁(Ⅲ)催化H2O2氧化吡咯红Y的反应，建立了一种测定柠檬酸的动力学荧光分析法。方法的线性范围为0．12-2．4μg/mL，检出限为0．05μg/mL。将方法用于汽水中柠檬酸的测定，回收率为97％-106％。     

A quick method for the simultaneous determination of ascorbic acid and sorbic acid in fruit juices by capillary zone electrophoresis

A method of quickly determining ascorbic acid and sorbic acid by capillary zone electrophoresis with ultraviolet detection was developed. The choice of background electrolyte, wavelength, injection time and applied voltage were discussed. Ascorbic acid and sorbic acid were well separated in 80 mmol L⁻¹ boric acid-5 mmol L⁻¹borax (pH = 8.0) in 5 min at the detecting wavelength of 270 nm. Under the optimum condition, the method has linear ranges of 2.54-352.00 mg L⁻¹ for ascorbic acid and 1.08-336.39 mg L⁻¹ for sorbic acid with the detection limit of 1.70 mg L⁻¹ for ascorbic acid and 0.54 mg L⁻¹ for sorbic acid, respectively. Other organic acids in fruit juices have no effect on the detection. This method is very feasible and simple and can be used to detect ascorbic acid and sorbic acid in fruit juices.     

Printed electrochemical sensor for ascorbic acid determination

Simple, strip-type sensors based on 7,7,8,8-tetracyanoquinodimethane-modified graphite were prepared using screen printing techniques. The electrochemical strips operated at low potentials [50 mV at pH 7.0 or 100 mV at pH 4.8 vs. Ag/AgCl (printed)] and had a sensitivity of 3.5–7.1 μA 1 mmol^?1L-ascorbic acid. Determination of ascorbic acid concentration was achieved in 30 s and required samples of ca. 30 μl. The current output of the electrodes was found to be relatively insensitive to variations in pH over the range 5.0–8.5. Between 15 and 35 °C, the temperature coefficient was 2.7% °C^?1. The printed electrodes were suitable for single determinations but demonstrated adequate stability for periodic re-use. The ascorbic acid concentration in the juice of fresh fruit was determined using the electrochemical printed electrodes and a commercially available enzymatic test kit. Close agreement was observed between the two methods [r=0.9997 (n=12),slope=0.9798]. The limit of detection using the printed sensor for real samples was calculated as 4mg l^?1(22 μM).     

A quercetin-modified biosensor for amperometric determination of uric acid in the presence of ascorbic acid

The present work reports a quercetin-modified wax-impregnated graphite electrode (Qu/WGE) prepared through an electrochemical oxidation procedure in quercetin-containing phosphate buffer solution (PBS), for the purpose of detecting uric acid (UA) in the presence of ascorbic acid (AA). During modification quercetin was oxidized to the corresponding quinonic structure, and in the blank buffer solution the electrodeposited film exhibits a voltammetric response anticipated for the surface-immobilized quercetin. Retarding effect of the film towards the reaction of anionic species was found; therefore the pH of sample solutions was selected to ensure the analyte in molecular form. At suitable pHs the Qu/WGE shows excellent electrocatalytic effect towards the oxidation of both AA and UA, and separates the voltammetric signal of UA from AA by about 280 mV, allowing simultaneous detection of these two species. A linear relation between the peak current and concentration was obtained for UA in the range of 1-50 μM in the presence of 0.5 mM AA, with a detection limit 1.0 μM (S/N = 3). This sensor was stable, reproducible and outstanding for long-term use.     

Flow-injection spectrophotometric determination of ascorbic acid by reduction of vanadotungstophosphoric acid

Ascorbic acid may be determined spectrophotometrically at 360 nm based on reduction of vanadotungstophosphoric acid using flow-injection analysis. The carrier stream was distilled water and the reagent streams were buffer solution (pH 3.0), 1.735 × 10^?3 M dodecatungstophosphoric acid and 1.735 × 10^?3 M sodium vanadate. The injection rate was 80 h^?1. The calibration graph was linear up to 80 μg ml^?1 ascorbic acid and the relative standard deviation for the determination of 20 μg ml^?1 ascorbic acid was 1.5% (n=10). The detection limit was 1.0 μg ml^?1 ascorbic acid, based on an injection volume of 250 μl. The system was applied to the determination of ascorbic acid in vitamin C tablets.     

流动注射抑制电化学发光法测定维生素C

将在线恒电流电解产生ClO-与Luminol构成了较强的化学发光体系,基于维生素C对该化学发光体系有强抑制作用,结合流动注射技术,建立了测定维生素C的流动注射抑制电化学发光新方法.该方法在维生素C的浓度为2.0×10-10～1.5×10-8 mmol/mL之间分段回归,呈良好的线性,检出限达到5.0×10-11 mmol/mL.     

Layer-by-layer thin film-coated electrodes for electrocatalytic determination of ascorbic acid

Multilayer thin films composed of poly(allylamine hydrochloride) (PAH) and carboxymethyl cellulose (CMC) have been prepared on the surface of a gold (Au) disk electrode by a layer-by-layer deposition of PAH and CMC and ferricyanide ions ([Fe(CN)₆]³⁻) were confined in the film. [Fe(CN)₆]³⁻ ions can be successfully confined in the films from weakly acidic or neutral [Fe(CN)₆]³⁻ solutions, while, in basic solution, [Fe(CN)₆]³⁻ ion was not confined. The [Fe(CN)₆]³⁻ ion-confined Au electrode showed clear redox peaks in the cyclic voltammogram around 0.35 V versus Ag/AgCl. The amounts of [Fe(CN)₆]³⁻ ions confined in the films depended on the thickness of the films or the number of layers in the LbL films. The [Fe(CN)₆]³⁻ ion-confined Au electrode was used for electrocatalytic determination of ascorbic acid in the concentration range of 1-50 mM.     

Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid

Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l⁻¹ was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l⁻¹ ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid–base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2–8% w v⁻¹ of acetic acid with a relative standard deviation of 4.8% (5.0% w v⁻¹ acetic acid, n=11) was obtained. Sample throughputs of 60 h⁻¹ were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.