共查询到20条相似文献,搜索用时 15 毫秒
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Wallans Torres Pio dos Santos Edimar Gledison Nascimento de Almeida Humberto Eustáquio Alves Ferreira Denise Tofanello Gimenes Eduardo Mathias Richter 《Electroanalysis》2008,20(17):1878-1883
The present work reports a simple and quick strategy for simultaneous determination of paracetamol (PC) and ascorbic acid (AA) in pharmaceutical formulations using flow injection method with multiple pulse amperometric detection. The method allows the resolution of the mixture without chemical pretreatment of the sample or electrode modification or the use of chemometric techniques for data analysis. The compounds are detected by applying four sequential pulses (waveform) in function of time to a three‐electrode amperometric system that uses a wall‐jet cell with gold as working electrode. AA is direct detected at +0.40 V and PC is indirectly detected at 0.0 V by the reduction (desorption) of the oxidation product (N‐acetyl‐p‐benzoquinoneimine) electrochemically generated at +0.65 V. The fourth potential pulse (?0.05 V) is applied for the complete regeneration (cleaning) of the gold electrode surface. The linear response range was optimized between 5 and 24 mg L?1 for AA and 50 and 240 mg L?1 for PC. The difference between the two responses ranges (10‐fold) present correlation with the concentration of these compounds in two different pharmaceutical formulations available in the Brazilian market. The analytical frequency was calculated in 60 injections per hour. The use of the proposed methodology for PC quantification in the presence of higher AA concentrations was also carried out. Using the standard addition method, it was possible to detect PC in trace levels (LD=0.2 mg L?1) in the presence of 880‐fold more of AA (176 mg L?1). 相似文献
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抗坏血酸的双安培流动注射分析 总被引:30,自引:0,他引:30
将流动注射双安培法应用于两种物质的不可逆电对体系。在两电极电位差即外加电压为零时,使用经过在0.01mol/LNaOH溶液中1.5V恒电位预处理的双铂丝电极,基于Vc的氧化和溶解氧的还原,拟定了流动注射双安培法测定Vc的新方法。Vc氧化电流与其浓度在1×10~(-5)mol/L-2×10~(-3)mol/L范围内呈线性关系,检测限为8×10~(-6)mol/L;两铂电极经预处理后,灵敏度增加4~6倍;连续进样24次,电流值RSD=1.58%。用本方法测定了Vc片剂和柑桔中Vc的含量,得到满意结果。 相似文献
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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. 相似文献
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磷钼钨三元杂多酸光度法测定药物中的抗坏血酸 总被引:2,自引:0,他引:2
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。 相似文献
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《Analytical letters》2012,45(5):941-951
ABSTRACT A simple and accurate procedure for indirect spectrofluorimetric determination of glycerol and ethylene glycol in aqueous media was developed. Alizarin Navy Blue can be oxidized by potassium periodate to produce a fluorescent compound, that can be detected fluorimetrically (λex = 370 nm, λem = 516 nm) by a flow through method. Glycerol and ethylene glycol react with periodate decreasing its concentration and thus the forming the basis for an indirect determination of these compounds. The influence of acid concentration, reagent concentration and manifold variables were studied. For glycerol and ethylene glycol linear calibration curves were obtained in the ranges of 4.8 × 10-7 – 8.7 × 10-5 M and 6.4 × 10-7 – 8.7 × 10-5 M, respectively. The limit of detection (defined as the concentration that gives a signal three times the standard deviation of the background signal) for glycerol and ethylene glycol was 3.2 × 10-7 M and 4.3 × 10-7 M, respectively. The proposed method was applied for determination of glycerol and ethylene glycol in synthetic and real samples. The results obtained were satisfactory. 相似文献
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于pH 7.0的磷酸盐缓冲介质中,CTMAB+及I3-离子间借静电引力形成离子缔合物,可将其浮选入5.0 mL苯中,此缔合物在溶剂中,于365 nm处有吸收峰,较简单的I3^-离子在相同条件下的吸收峰(350 nm)红移了15 nm。在此溶液体系中存在抗坏血酸时使离子缔合物产生褪色反应,且在抗坏血酸浓度在25μg/50 mL以内时与吸光度的降低值(ΔA)间呈线性关系。在抗坏血酸浓度为6.0μg/50 mL时连续测定6次,所得结果的RSD为1.2%,回收率在96%-101%之间。 相似文献
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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 λmax, 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. 相似文献
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流动注射在线光化学荧光法测定药物制剂中叶酸的含量 总被引:7,自引:0,他引:7
叶酸接受紫外光照后可转变成最大激发波长为274nm、最大发射波长为466nm的强荧光化合物。对光化学反应介质进行考察,发现在NaC03—NaHC03缓冲体系中所产生的光化学荧光最强,据此建立了流动注射在线光化学荧光分析法。试样在水载流的携带下与PH9.5的Na2C03—NaHC03缓冲溶液汇流后,通过一个盘绕在6—W低压汞灯上的PTFE编结式光化学反应器。在反应器中所生成的荧光化合物直接通入荧光计的流通池测定荧光强度。在最佳条件下,动态线性范围可达0.001-4mg/L,检测限为0.16μg/L,采样速率达80/h,11次测定浓度分别为0.01和0.1mg/L的叶酸标准溶液所得到的RSD分别为1.0%和0.2%。所建立的方法已成功地用于片剂中叶酸含量的测定。 相似文献
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A novel flow injection procedure has been developed for the determination of tannic acid based on the inhibition of the chemiluminescences
in luminol-H2O2-Manganese tetrasulfonatophthalocyanine (MnTSPc) system by tannic acid. The method is simple, rapid and sensitive with a detection
limit of 8 × 10−10 mol·L−1 and a linear range of 7 × 10−9–5 × 10−6 mol·L−1. The relative standard deviation is 1.9% for eleven measurements of 5 × 10−7 mol·L−1 tannic acid. The method has been successfully applied to the determination of tannic acid in real Chinese gall and hop pellets
samples. 相似文献
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《Analytical letters》2012,45(9):1131-1142
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 δmax 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%. 相似文献
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《Electroanalysis》2003,15(14):1171-1176
A silica sol‐gel glass‐coated ferricyanide‐doped Tosflex‐modified screen‐printed electrode (designated as SG/FeCN‐Ts/SPE) was used for the mediated oxidation of ascorbic acid in neutral pH. The sol‐gel overlayer was found to stabilize the Fe(CN) ‐Tosflex system without any foul‐off and deterioration behavior through chemical interaction between the hydrophilic sites of Tosflex and oxy‐ and/or ‐hydroxy surface functional groups of silicate. The electrochemical mediation of ascorbic acid was found to follow the Michaelis‐Menten kinetic pathway. The SG/FeCN‐Ts/SPE was very stable for repetitive measurements by flow injection analysis at 0.3 V (vs. Ag/AgCl). A linear calibration plot was obtained for ascorbic acid determination up to 300 μM with sensitivity and detection limit (S/N=3) of 2.85 nA/μM and 46 nM, respectively. The system also showed tolerable interference to uric acid, urea and carbohydrates and was used for the determination of ascorbic acid in human urine, clinical tablet and apple juice. 相似文献
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《Analytical letters》2012,45(15):3239-3252
ABSTRACT Potential dependent inhibition and enhancement effects of gallic acid on the electrochemiluminescence (ECL) of luminol in alkaline solutions were found. On the basis of the enhancement effect, a flow injection method was developed for the determination of gallic acid. The method was simple, convenient and sensitive. A detection limit of 1.8×10?8 mol/L, linear range of 3.0×10?8 - 1.0×10?4 mol/L, relative standard deviation of 1.0% for eleven measurements of 5.0×10?6 mol/L of gallic acid was found. This method was successfully applied to determine the content of gallic acid in Chinese gall (moshizi). 相似文献