克拉霉素与百里酚蓝荷移配合物的光度分析研究

利用克拉霉素与百里酚蓝在乙醇介质发生荷移反应,建立了荷移分光光度法测定克拉霉素含量的方法.结果表明,荷移反应生成1∶1型配合物,最大吸收波长为442 nm,表观摩尔吸光系数为ε=1.66×104L·mol-1·cm-1,克拉霉素测定线性范围为8.278～57.59 mg/L.     

Spectrophotometric and derivative spectrophotometric determination of nickel with hydroxynaphthol blue

The reaction of nickel(II) cation with hydroxynaphthol blue (HNB) in aqueous media at pH 5.2–6.0 results in a red complex that is stable for at least 2h. Beer's Law is obeyed up to 3.2 g/ml of nickel(II) with an apparent molar absorptivity of 1.38 × 10⁴l/mol/cm at 563 nm. This paper proposes procedures for nickel determination by ordinary and first-derivative spectrophotometry. The results demonstrate that the linear dynamic range is 0.08–3.20 g/ml with a limit of detection of 23 ng/ml for ordinary spectrophotometry, compared with 21–800 ng/ml and 6 ng/ml, respectively, for first-derivative spectrophotometry. Calcium(II), magnesium(II), barium(II), strontium(II), cadmium(II), lead(II), manganese(II), bismuth(III) and molybdenum(VI) ions do not interfere for at least 1001 mass ratios. The main interferents are cobalt(II), titanium(IV), aluminium(III), mercury(II) and copper(II). The interferences of titanium(IV), aluminium(III), zirconium(IV) and iron(III) can be masked by fluoride and mercury(II) and copper(II) with thiosulfate or thiourea. The derivative method is applied to nickel determination in standard brasses and the results demonstrate that there is no significant difference between the results and certified values at the 95% confidence level.     

Spectrophotometric determination of 6-aminopenicillanic acid using bromophenol blue and bromothymol blue

Two simple, selective and sensitive spectrophotometric methods are described for the determination of 6-aminopenicillanic acid (6-APA). The methods are based on the reaction of 6-APA with either bromophenol blue (BPB) or bromothymol blue (BTB), to give orange-red and green species, respectively. The coloured products are quantified spectrophotometrically at 625 and 616 nm for BPB and BTB, respectively. The optimization of the different experimental conditions is described. No interferences from different -lactams and common degradation products were observed in the determination of 6-APA using BTB, while flucloxacillin, dicloxacillin, adrenaline, vitamin C, urea and common degradation products in any percentage interfere on using BPB only. The BTB method was better than the BPB method, because of its wider range of determination (0.4–20 g ml^–1 vs. 0.4–7.2 g ml^–1 on using BPB), higher molar absorptivity and Sandell sensitivity (3.27 × 10³l mol^–1 cm^–1 and 0.099 g cm^–2 vs. 2.82 × 10³lmol^–1 cm^–1 and 0.115 g cm^–2), greater stability (3 and 10 days on using BTB and BPB, respectively) and better selectivity. The results were compared with those given by the Official United States Pharmacopeial XXI method.     

Spectrophotometric determination of thorium as molybdothoric acid with basic dyes

Color developments based on the ion-association complexes of molybdothoric acid with three basic dyes (BD), rhodamine B(RB), butylrhodamine B(BRB) and nile blue (NB), were investigated in aqueous acidic solution in the presence of poly(vinyl alcohol) (PVA). Their spectrophotometric behavior, such as the conditions suitable for the reactions and the effects of foreign ions, were thoroughly studied. The ThMoBD ratio in the complexes was found to be 1123. Their absorption maxima were at 570, 570 and 590 nm with apparent molar absorptivities of 3.50 × 10^–6, 3.63 × 10⁶ and 4.45 × 10⁶ dm³ mol^–1 cm^–1, respectively. Beer's law was obeyed up to 0.8, 0.8 and 0.7 g thorium per 25 ml, respectively. The detection limits (3) were 1.1, 1.8 and 3.4 ng ml^–1, respectively, and for 0.02 ug ml^–1 solution of thorium the relative standard deviations were 3.0, 2.9 and 1.5%, respectively (n = 11). The proposed methods were applied to the determination of trace amounts of thorium in some geological samples.     

Spectrophotometric determination of mebeverine hydrochloride

Three simple, sensitive and reproducible visible spectrophotometric methods (A-C) for the determination of mebeverine hydrochloride (MVH) in bulk samples and pharmaceutical formulations are described. Methods A and B are based on the formation of ion-association complexes between the drug and fast green FCF (FGFCF, _max 625 nm) or bromothymol blue (BTB, _max 405 nm). Method C is based on the formation of a molecular complex between the drug and cobalt thiocyanate (CTC, _max 625 nm). Regression analysis of Beer's plots showed good correlation in the concentration ranges 2–40, 2–25 and 100–600 g/ml for methods A, B and C respectively. No interference was observed from the usually existing additives in pharmaceutical formulations and the applicability of the methods was examined by analysing tablets containing MVH. Standard deviations were typically 0.75 mg per dose (RSD: 0.25–0.5%). Recoveries were 99.0–100.2%.     

耐尔蓝-高碘酸钾-溴代十六烷基吡啶-氨三乙酸体系催化动力学光度法测定锰

在增敏剂溴代十六烷基吡啶和活化剂氨三乙酸存在的条件下，锰（Ⅱ）对高碘敢钾氧化耐尔蓝的反应具有催化作用，据此建立了测定锰的新方法。该法具有很高的灵敏度和选择性。在最优化的实验条件下，其线性范围为O．4--5．6μg/L；检出限为0．054μg/L(n=8)；相对标准偏差为3．8％。用于水样、蔬菜样品中锰含量的测定，结果令人满意。     

IO3--I--亚甲基蓝-阿拉伯胶-聚乙烯醇体系分光光度法测定微量碘

在pH 3.8苯二甲酸氢钾-盐酸介质中,有阿拉伯胶和聚乙烯醇存在下,IO-3氧化I-生成I-3,I-3再与亚甲基蓝形成离子缔合物,缔合物的最大吸收波长为525 nm,表观摩尔吸光系数ε525＝1.32×105 L/(mol·cm),IO-3浓度在0～30 μg/25 mL范围内服从比尔定律. 方法用于碘盐和生物样品中碘的测定,结果满意.     

Spectrophotometric and titrimetric determination of gallium in minerals and ores using semimethylthymol blue

The composition, overall stability constant and molar absorptivity of the chelate of gallium(III) ion with semimethylthymol blue, SMTB, were determined spectrophotometrically in acetate buffer (pH 4.5–5). A violet Ga(SMTB) chelate was formed with logarithmic overall stability constant of 18.0±0.1 (I=0.1) and molar absorptivity of 4.25×10⁴l mol^–1cm^–1 (_max 580 nm). SMTB is proposed as a new reagent for the spectrophotometric determination of micro-molar amounts of gallium(III). The colour development depends on time, temperature, pH and buffer species. The interference of different cations, anions and organic acids on gallium(III) determination was also investigated. Beer's law was obeyed for 3.5–31.3 gGa(III)/25ml (0.14–1.25 g ml^–1). SMTB was used for the spectrophotometric determination of gallium in different grade minerals and ores and the results were of acceptable error and relative standard deviation. Comparison between the two suggested methods and atomic absorption spectrometry for Ga(III) determination was carried out.     

Study on the colour reaction of Te-KI-RhB system in the presence of PVA-OP

A new supersensitive spectrophotometric method for the determination of tellurium (IV) has been developed which is based on the formation of an ion-association complex with potassium iodide and rhodamine B (RhB) in the presence of polyvinyl alcohol (PVA) and polyethylene glycol octyl phenyl ether (OP). The molar absorptivity at 560 nm is 2.8 × 10⁶ 1 mol^–1 cm^–1. Beer's law is obeyed over the range of 20–70 ng/ml Te. The method has been applied successfully to determine tellurium in alloy, steel and some other samples.     

Electrocatalytic oxidation of NADH at glassy carbon electrodes modified with an electropolymerized film of nile blue A

The kinetic parameters for the electrocatalytic oxidation of di-hydronicotiamide adenine dinucleotide (NADH) at glassy carbon electrodes modified with an electropolymerized film of nile blue A (PNB) have been determined based on rotating disk electrode measurements. The rate constant for the chemical reaction between NADH and PNB is strongly influenced by NADH concentration and the pH value of solution, and it decreases with increasing NADH concentration, indicating that the electrocatalytic process proceeds via the formation of an intermediate of charge-transfer complex between NADH and PNB.     

十二烷基苯磺酸钠-硫酸耐而蓝体系的共振瑞利散射光谱及其分析应用

提出了共振瑞利散射法(RRS)测定十二烷基苯磺酸钠(SDBS)的新方法。在pH为1.98～3.29的B-R缓冲溶液中,硫酸耐而蓝与SDBS结合生成离子缔合物,使溶液共振瑞利散射(RRS)增强,其最大散射峰位于760 nm,另在533 nm、400 nm有两个较弱的散射峰。SDBS的浓度在0.04～1.6 mg/L范围内,与RRS强度有良好的线性关系,对SDBS的检出限(3σ)达0.018 mg/L。研究了适宜的反应条件和影响因素,表明该方法灵敏、稳定。用于环境水样中阴离子表面活性剂含量的测定,回收率为95.9%～106.7%。     

亚甲基蓝光度法测苯唑西林

在pH8.6～9.8的条件下,亚甲基蓝与苯唑西林反应生成蓝色离子缔合物。体系的最大吸收波长位于606nm,线性范围为0～4.0mg/L,表观摩尔吸光系数为2.60×104L·mol-1.cm-1,探讨了适宜的反应条件、方法的精密度及可靠性。方法已用于药物中阿莫西林的测定。     

I-3-MB-AES体系分光光度法测定面粉中过氧化苯甲酰

在磷酸介质中,过氧化苯甲酰(BPO)氧化I<'->离子形成I<'-><,3>络阴离子,I<'-><,3>络阴离子进一步与亚甲基蓝形成离子缔合物,在烷基聚氧乙烯醚硫酸钠(AES)中,缔合物呈清亮的蓝紫色溶液,以试剂空白为参比,最大吸收波长位于530nm,吸光度A与过氧化苯甲酰浓度呈线性关系,BPO含量在2.0×10<'-...     

用耐尔蓝和高碘酸盐催化光度法测定痕量铱(Ⅳ)

研究了在弱酸性介质中,利用铱（Ⅳ）催化高碘酸钾氧化耐尔蓝（ＮＢ）形成桃红色产物,建立了催化光度法测定痕量铱的新方法。方法的线性范围为４．０￣４０μｇ／Ｌ;检出限为４．０μｇ／Ｌ,对４０μｇ／Ｌ Ｉｒ（Ⅳ）测定的ＲＳＤ为２．０２％。本法满意地用于某些矿石和冶金产品中铱的测定。     

酸性铬兰K分光光度法测定血红蛋白

在pH 3.2的Clark-Lub’s缓冲溶液中,酸性铬兰K与血红蛋白发生反应,使体系吸光度增大,在375 nm处的吸光度增加值与血红蛋白的加入量成正比,据此建立了测定血红蛋白的分光光度法。探讨了测定血红蛋白的最佳条件和干扰情况,方法的线性范围0～112μg/mL,表观摩尔吸光系数ε375为4.7×105L.mol-.1cm-1,方法已用于动物血液和人尿液中血红蛋白含量的测定。     

苯胺蓝增色光度法测定食盐中的碘

在H2SO4介质中,KIO3与苯胺蓝反应增色程度与IO3-量在一定范围内呈线性关系,从而建立了增色光度法测定碘的新方法.实验结果表明,该体系最大吸收波长为603 nm,IO3-在0.91～4.55 μg/L范围内符合比耳定律,表观摩尔吸光系数为5.00×105 L·mol-1·cm-1.本法可直接测定食盐中的碘.     

依文思蓝光度法测定阿昔洛韦及其分析应用

在pH 5.74 HAc-NaAc缓冲介质中, 阿昔洛韦(ACV)与依文思蓝(EB)反应形成离子缔合物, 溶液颜色发生明显改变, 最大褪色波长为638 nm. 在此波长处, 阿昔洛韦的浓度与褪色程度呈良好线性关系, 从而建立测定阿昔洛韦的光度法. 在最大褪色波长处, 阿昔洛韦的浓度在0～2.01×10-5 mol/L范围内遵守比尔定律, 表观摩尔吸光系数1.71×104 L·mol-1·cm-1, 检出限为7.47×10-7 mol/L. 方法具有较高的灵敏度和良好的选择性, 可用于实际药品、血浆及尿液中阿昔洛韦的测定.     

奈替米星与依文思蓝的光度分析研究

硫酸奈替米星是半合成的一种较新的氨基糖苷类抗生素,由西梭米星乙酰化而成,它不但全面保留了西梭米星的体内抗菌活性,同时提高了西梭米星对钝化酶的耐受性,其抗菌谱广,活性高,耳、肾毒性较其他同类药小,现已广泛用于国内外临床[1-3]。对奈替米星的测定方法,目前已报道的主要有     

溴酚蓝光度法测定马来酸罗格列酮的含量

在pH 4.50的Britton-Robinson(B-R)缓冲溶液中,溴酚蓝(BPB)与马来酸罗格列酮(ROM)反应,形成1∶1的离子缔合物,溶液颜色明显发生改变,最大吸收波长为434 nm,同时在波长590 nm处产生负吸收.在590 nm处,马来酸罗格列酮浓度分别在0～1.70×10-5 moL/L范围遵循比尔定律,表观摩尔吸光系数ε590为4.51×104 L/(mol·cm),检出限为2.60×10-7 mol/L.方法可用于分析检测马来酸罗格列酮的含量.     

Spectrophotometric method for the determination of demeclocycline using sodium molybdate as analytical reagent

By means of spectroscopic methods it has been found that demeclocycline reacts with molybdate ions forming a complex compound [MoO₃HDMTC]^2–. The relative stability constant of this compound has been determined by applying spectrophotometric methods. Under optimum conditions for complex formation a very sensitive spectrophotometric method for the estimation of demeclocycline in the concentration range 5.0–35.1 g/ml is proposed. The detection limit of the method is 2.5 g/ml of demeclocycline. The relative standard deviation (n=10) varies between 0.76% and 1.46%. The method proved to be accurate and sensitive for the analysis of the demeclocycline content in tablets.