磷钼钨三元杂多酸光度法测定药物中的抗坏血酸

研究了抗坏血酸与磷钼钨三元杂多酸的显色反应,提出了借磷钼钨杂多蓝测定抗坏血酸的分光光度法.最大吸收波长为730nm,抗坏血酸在0.08～10mg/L范围内线性良好.回归方程为A=1.05×10⁴C+0.017,线性相关系数γ=0.9995,表观摩尔吸光系数ξ₇₃₀=1.05×10⁴L·mol^-1·cm^-1,方法检出限为0.04mg/L,回收率为94～102%,相对标准偏差≤1.5%(n=8).本方法由于钨钼的混合配位增强了氧化能力,较之二元杂多酸的方法,省去了水浴加热等操作,只需在室温下反应30min,吸光值至少可稳定6h.过量的黄色杂多酸可加入适量的氢氧化钠溶液分解,从而获得色泽纯正的高灵敏度显色体系.     

磷钼钨三元杂多酸光度法测定药物中的抗坏血酸

研究了抗坏血酸与磷钼钨三元杂多酸的显色反应，提出了借磷钼钨杂多蓝测定抗坏血酸的分光光度法。最大吸收波长为７３０ｎｍ，抗坏血酸在０．０８～１０ｍｇ／Ｌ范围内线性良好。回归方程为Ａ＝１．０５×１０４Ｃ＋０．０１７，线性相关系数γ＝０．９９９５，表观摩尔吸光系数ξ７３０＝１．０５×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，方法检出限为０．０４ｍｇ／Ｌ，回收率为９４～１０２％，相对标准偏差≤１．５％（ｎ＝８）。本方法由于钨钼的混合配位增强了氧化能力，较之二元杂多酸的方法，省去了水浴加热等操作，只需在室温下反应３０ｍｉｎ，吸光值至少可稳定６ｈ。过量的黄色杂多酸可加入适量的氢氧化钠溶液分解，从而获得色泽纯正的高灵敏度显色体系。     

Spectrophotometric Determination of Trace Amounts of Ascorbic Acid

Abstract

Colourless silver-gelatin complex is quantitatively reduced by ascorbic acid to yellow silver sol in water within the pH range 7.5–10.0 at room temperature. The determination of 1–10μg/ml of ascorbic acid is possible at 415 nm in the presence of glycine, alanine, fructose, sucrose, citric, tartaric, oxalic, malic, succinic acids and also in the presence of various reducing agents. The molar absorptivity of ascorbic acid at the δ_max is found to be 21500 lit mol^?1 cm^?1 and the Sandell sensitivity of the sol is 8.18x10^?3 μg ascorbic acid cm^?2 for 0.001 absorbance. The relative standard deviation is ±0.22% and the confidence limit (20 determinations, 95%) being 8.806±0.0093%.     

A Comparative Study on Spectrophotometric,Conductometric and Potentiometric Determination of Ascorbic Acid

Abstract

A comparison has been made on the selectivity, accuracy and precision of spectrophotometric, conductometric and potentiometric methods for the determination of ascorbic acid in water which is based on the reduction of gold(III) ion by ascorbic acid. Gold(III) ion forms a complex with gelatin in alkaline medium which on reduction with ascorbic acid produces coloured gold sol. The sol shows an absorption maximum at 540 nm with molar absorptivity of 2.3×10^?3litre mol^?1 cm^?1 and the Sandell's sensitivity of 7.6 × 10^?2 μgcm^?2. The relative standard deviation is 0.22% and the confidence limit (20 determinations, 95%) is 2.0 ± 0.009%. To examine the extent of sensitivity of the spectrophotometric method the proposed method is compared with the sensitivities of the conductometric and potentiometric methods.     

固蓝盐B分光光度法测定药物中抗坏血酸

探讨了一种简便的选择性高的药物中抗坏血酸的测定方法。该方法是基于在酸性介质中抗坏血酸和固蓝盐B的反应,产物的最大吸收为420nm.摩尔吸光系数为1.31×10~4L·mol~(-1)·cm~(-1).方法已应用于某些药物中抗坏血酸的测定,结果与碘量法一致,回收率为98.4％～105％,相对标准偏差低于3.7％。     

A Spectrophotometric Determination of Ascorbic Acid

A new, simple and sensitive method for the spectrophotometric indirect determination of ascorbic acid in fruits, beverages, and pharmaceuticals is described. In this method, the ascorbic acid reduces Cu²⁺ to Cu⁺ and reacts with 2,9‐dimethyl‐1,10‐phenanothroline (neucoproine) to form Cu (neucoproine)⁺ complex, and it was extracted with N‐phenylbenzimidoylthiourea (PBITU) in chloroform. The apparent value of molar absorptivity of the complex in terms of ascorbic acid is (3.52) × 10⁴ L mole^?1 cm^?1 at λ_max, 460. The detection limit of ascorbic acid is 40 μg L^?1 and the method obeys Beer's law over the concentration range of 0.1–4.0 μg mL^?1. The proposed method was successfully applied for the determination of ascorbic acid in various samples. The validity of the present method was checked by the flow injection analysis (FIA) method.     

Spectrophotometric Determination of Methotrexate and in Pharmaceutical Formulations

Abstract

Methotrexate, 4-amino-10-methyl folic acid, is one of the drugs belonging to the folic acid antagonists that is widely used for the treatment of cancer and psoriasis ^{1, 2}     

饮料、甜橙、药片和尿液中维生素C的流动注射分析——2,6-二氯吲哚酚光度法

流动注射2,6-二氯吲哚酚光度法测定维生素C具有灵敏,快速的特点,检出限为0.5μg/ml,分析速度120样/h,取Vc 40μg/ml时测量的相对标准偏差为±0.5％。测定各类样品中Vc含量获得较好的结果。     

Resin Bead Detection and Spectrophotometric Determination of Ascorbic Acid in Pharmaceutical Preparations Using m-Dinitrobenzene

Abstract

A colorimetric reaction has been studied for the detection and determination of ascorbic acid in samples at the microgram level. the method is simple, rapid, and sensitive, the ascorbic acid was detected using resin beads and determined spectrophotometrically using m-dinitrobenzene in formaldehyde. the detection limit was 10μg. Beer's law is obeyed in the concentration range of 2 – 50μg/ml of ascorbic acid.     

Kinetic and Spectrophotometric Determination of Thioctic Acid in Bulk and Pharmaceutical Formulations

Three simple and sensitive spectrophotometric methods were developed for the determination of thioctic acid in bulk and in its pharmaceutical preparations using iron(III) as an oxidizing agent. Method A is based on kinetic investigation of oxidation reaction of the drug with iron(III) and a subsequent chelation of the produced iron(II) with ferricyanide to form prussian blue colored product at room temperature for a fixed time of 15 minutes at 750 nm. Methods B and C are based on oxidation of the studied drug with iron(III). The equivalent iron(II) produced is allowed to react with either o‐phenanthroline or bipyridyl to give colored species measurable at 510, 522 nm, respectively. Regression analysis of Beer‐Lambert plots showed a good correlation in the concentration ranges of 0.4–4 μg/mL with a detection limit of 0.095 μg/mL for method A and 0.5–5 μg/mL with detection limits 0.137 and 0.127 for method B and C, respectively. The three methods were successfully applied for the determination of the drug in its dosage forms. The percentage recoveries were 99.88 ± 1.40, 99.98 ± 1.26 and 100.64 ± 1.07, respectively.     

The Influence of Gold Nanoparticles on Simultaneous Determination of Uric Acid and Ascorbic Acid

A three-dimensional L-cysteine (L-cys) monolayer assembled on gold nanoparticles (GNP) providing simultaneous detection of uric acid (UA) and ascorbic acid (AA) was studied in this work. The cyclic voltammetry demonstrated that, at a bare glassy carbon electrode (GCE) or planar gold electrode, the mixture of UA and AA showed one overlapped oxidation peak; whereas when the electrode was modified with GNP, the oxidation peaks for UA and AA were separated. While a GNP modified electrode was further modified with L-cys monolayer (L-cys/GNP/GCE), namely, three-dimensional L-cys monolayer, a better separation for UA and AA response was obtained. Interestingly, the L-cys monolayer-modified planar gold electrode presented a block effect on the oxidation of AA, which was facilitated by the three-dimensional L-cys monolayer attributed to its distinct structure. The pH of solution presented a noticeable effect on the separation of UA and AA at GNP modified electrodes with or without L-cys monolayer. Wide concentration ranges from 2 × 10^?6?1 × 10^?3 M to UA and 2 × 10^?6?8 × 10^?4 M to AA could be obtained at L-cys/GNP/GCE.     

Kinetic Spectrophotometric Determination of Ascorbic Acid in Pharmaceutical Samples by Oxidation of Ponceau 4R by Hydrogen Peroxide

A new sensitive and simple kinetic method is developed for determination of traces of ascorbic acid based on its activated effect on oxidation of trisodium‐2‐hydroxy‐1‐(4‐sulphonato‐1‐naphthylazo)naphthalene‐6,8‐disulphonato (red artificial color Ponceau 4R) by hydrogen peroxide, in the presence of Cu(II) as catalyst, in borate buffer. The reaction is followed spectrophotometrically by tracing the oxidation product at 478.4 nm within 1 min after addition of H₂O₂. The optimum reaction conditions are: borate buffer (pH = 11.00), Ponceau 4R (9.6·10^?6 mol/L), H₂O₂ (2·10^?2 mol/L), Cu(II) (8·10^?7 mol/L) at 22 °C. Following this procedure, ascorbic acid can be determined with a linear calibration graph up to 1.76 ng/mL and a detection limit of 0.28, based on 3S criterion. The relative error ranges between 6.77‐1.66% for the concentration interval of ascorbic acid 1.76‐17.61 ng/mL. The effects of certain foreign ions upon the reaction rate were determined for an assessment of the selectivity of the method. The method was applied for determination of ascorbic acid in pharmaceutical samples, and spectrophotometric method was used like an comparative method.     

2nd and 3rd Order Derivative Spectrophotometric Determination of Ascorbic Acid in Soft Drinks

Abstract

A method is developed for the 2nd and 3rd order derivative spectrophotometric determination of 0.5–6 and 0.5–7 μ.ml^?1 of ascorbic acid, respectively. For its determination in soft drinks a blank solution is prepared from the soft drink to be analyzed in order to avoid the interference from the other additives and colouring matter present.     

Simultaneous Differential Pulse Voltammetric Determination of Ascorbic Acid and Caffeine in Pharmaceutical Formulations Using a Boron‐Doped Diamond Electrode

A cathodically pretreated boron‐doped diamond electrode was used for the simultaneous anodic determination of ascorbic acid (AA) and caffeine (CAF) by differential pulse voltammetry. Linear calibration curves (r=0.999) were obtained from 1.9×10^?5 to 2.1×10^?4 mol L^?1 for AA and from 9.7×10^?6 to 1.1×10^?4 mol L^?1 for CAF, with detection limits of 19 μmol L^?1 and 7.0 μmol L^?1, respectively. This method was successfully applied for the determination of AA and CAF in pharmaceutical formulations, with results equal to those obtained using a HPLC reference method.     

Flow Injection Analysis Determination of Ascorbic Acid with Spectrofluorimetric Detection

Abstract

A flow injection system for the fluorescence determination of low level of ascorbic acid is proposed. The method is based on the rapid oxidation of ascorbic acid by thallium(I). The fluorescence signal at 419 nm is proportional to the amount of ascorbic acid in the range of (1.4–28.0) × 10^?7 mole. The relative standard deviations for ten replicate measurements of 1.4 × 10^?6 mole of ascorbic acid was 1.3%. The sample rate of 45 ± 5 sample per hour was achieved. The usefulness of the method was tested in the determination of ascorbic acid in fruit juices and vitamin C tablets.     

Disposable Stochastic Dot Sensors for the Assay of Ascorbic Acid in Pharmaceutical Samples,Beverages, and Biological Fluids

Eight disposable stochastic dot sensors based on porphyrins and modified diamond or carbon pastes were employed for the assay of ascorbic acid in pharmaceutical, beverages, and biological samples. The advantage of using such sensors for the assay of ascorbic acid is the possibility of qualitative and quantitative assay of ascorbic acid in one run of the experiment. The covered linear concentration range for these sensors was between 10^?14 and 10^?5 mol/L with high sensitivities. The proposed dot sensors were used reliably (RSD < 1%) for the assay of ascorbic acid from different samples for more than 6 months, with a recovery higher than 92.00%.     

Electrochemical Behaviors of Ascorbic Acid and Uric Acid in Ionic Liquid

Cyclic voltammetric measurements at platinum electrode have been carried out to investigate the electrochemical oxidation of ascorbic acid and uric acid in ionic liquid, [bmim][BF₄]. It is important that a typical redox couple of ascorbic acid was obtained and it is oxidized to dehydroascorbic acid in [bmim][BF₄]. However, there is no electron-transfer for uric acid and no electrochemical oxidation carried out in the same ionic liquid. It provides a new way to eliminate the interfering between ascorbic acid and uric acid in the study of the electrochemical behaviors for them.     

Determination of Paracetamol in Presence of Ascorbic Acid in Pharmaceutical Products by Scanning Electrochemical Microscopy

The selective amperometric determination of paracetamol in pharmaceutical formulations containing ascorbate was achieved by removing the interfering species in the diffusion layer created between a platinum substrate and a disc microelectrode in a Scanning Electrochemical Microscopy (SECM) configuration, while the target analyte was kept unconsumed. After complete depletion of ascorbate, paracetamol was detected at the SECM tip in a free‐interference solution zone. The influence of the substrate potential and the gap distance on the efficiency of ascorbate removal was systematically examined. The effectiveness of the device towards the determination of paracetamol in pharmaceutical samples was evaluated and under optimal conditions the results obtained agreed well with the labeled value.