高效液相色谱-串联质谱法同时测定染发剂中的1-萘酚和2-萘酚

提出了同时测定染发剂中1-萘酚和2-萘酚的高效液相色谱-串联质谱分析方法。染发剂样品经甲醇-水(1+1)混合液萃取,ProElut PLS固相萃取小柱净化,净化液吹氮蒸干后残渣用甲醇溶解并定容为1mL。此溶液经Agilent ZORBAX SB-C18色谱柱(2.1mm×150mm,3.5μm)分离,用不同体积比混合的乙腈和水梯度洗脱,采用电喷雾负离子模式多反应监测。1-萘酚和2-萘酚的线性范围均为0.05~10.0mg·L-1,检出限(3S/N)均为0.05mg·kg-1,测定下限(10S/N)均为0.2mg·kg-1。方法应用于测定实际样品中上述两化合物。以空白样品作基体加入混合标准溶液做回收试验,测得回收率在82.5%~102%之间,测定值的相对标准偏差(n=10)在6.3%~11%之间。     

导数-可变角同步荧光法用于1-萘酚和2-萘酚的同时测定

同步扫描和导数光谱法是两类很有用的荧光分析新技术。固定波长或恒能量同步荧光法和导数技术的结合可进一步提高光谱分辨率和排除基体干扰。本文将导数技术和可变角同步荧光法结合起来,用于1-萘酚和2-萘酚的同时分析,效果良好。研究表明,导数-可变角同步荧光法可望发展为荧光分析复杂样品的新技术。     

pH值对α-萘酚、β-萘酚与β-环糊精包结常数影响的研究

利用荧光法研究了不同pH值条件下萘酚的荧光性质,并用双倒数法测定了α-萘酚、β-萘酚与β-环糊精包结物在不同pH值的包结常数.实验表明,随pH值由小到大的变化,两种萘酚的包合作用逐渐减弱,说明包合物形成过程中疏水作用和氢键起重要作用.     

非催化条件下合成1-苯甲酰基-2-萘酚

以2-萘酚和三氯甲苯为起始原料,异丙醇水溶液作溶剂,非催化条件下合成了1-苯甲酰基-2-萘酚。考察了三氯甲苯用量、醇、水和异丙醇的体积比、溶剂用量及回流反应时间对产率的影响。确定较佳工艺条件为:2-萘酚50 mmol,三氯甲苯60 mmol,异丙醇水溶液18 mL(V水∶V异丙醇=1∶5),回流反应时间2 h,1-苯甲酰基-2-萘酚收率达74%。异丙醇经回收后可重复利用。产品结构经IR,1H NMR,13C NMR及元素分析进行了表征。     

共振瑞利散射光谱法同时测定α-萘酚和β-萘酚异构体

在硼砂-HCI(pH=8.2)的水溶液中,α-萘酚(α-N)和β萘酚(β-N)分别与卢一环糊精(β-CD)形成包合物,对共振瑞利散射光谱(RRS)有很强的增敏作用.实验发现.α-N和β-N两种包合物的RRS光谱在320hm处有等强度的等散射点,β-N的包合物在338nm处出现一个突出尖峰,经偏振实验证实是共振荧光峰,而两者在470nm处的共振瑞利散射峰形和增强趋势一致,且具加和性.故可在470nm处测定萘酚的总量,再在338nm处以"同原射线计量法"测定β-N和α-N的含量.在470nm处测定萘酚总量实验的线性范围为5.0×10-63.6×10-4mol/L,最低检出限为2.0×10-6mol/L,RSD为3.5%.在338nm处测定β-N和α-N含量的线性范围均为5.0×10-6～3.1 X 10-4mol/L,最低检出限分别为1.6×10-6mol/L和1.8×10-6mol/L.RSD分别为3.7%和3.6%.测定的选择性较好,据此可对合成样品进行同时测定和对α-萘酚试剂的纯度分析,结果令人满意.     

1,1′-联-2-萘酚的合成新进展

1,1′-联-2-萘酚是具有C2轴不对称联芳香族化合物,已在不对称合成、分子识别、新材料合成等领域有着广泛的应用。文章综述了1,1′-联-2-萘酚的基本性能、应用以及国内外最常用与最新的合成方法。     

β-萘酚α位反应的研究进展

萘酚是有机合成中一种重要的合成子,其α位化学性质活泼,可参与多种化学反应,受到了化学家的广泛关注. β-萘酚的α位可以发生多种化学转化,如烷基化、芳基化、环化、胺化和卤化等,利用这些化学反应可以构建结构多样化且具有不同生物活性的萘酚衍生物.这些萘酚衍生物既可以作为天然活性药物的关键骨架,也可以用于制备化学合成中的重要中间体.基于近年来β-萘酚α位的化学反应层出不穷,主要从β-萘酚α位碳-碳键和碳-杂键(C—N,C—O, C—X, C—S, C—P)的构建来对β-萘酚α位的相关反应进行了综述.     

硫酸氢钾催化一锅法合成1-乙酰胺烷基-2-萘酚

以硫酸氢钾为催化剂,在无溶剂条件下催化2-萘酚和乙酰胺分别与苯甲醛、对硝基苯甲醛、水杨醛、茴香醛、香兰素等五种芳香醛的三组分反应,利用一锅法合成了系列1-乙酰胺烷基-2-萘酚.以1-乙酰胺基苯甲基-2-萘酚(AAN)的合成为模板反应考察了催化剂用量、反应温度、原料配比及反应时间等因素对产物收率的影响.结果表明,硫酸氢钾催化合成AAN反应的适宜条件为:n(2-萘酚)∶n(苯甲醛)∶n(乙酰胺)∶n(硫酸氢钾)=1∶1.2∶1.2∶0.05,90℃下反应40min,AAN的收率达92.1%.硫酸氢钾对其他四种反应也有较理想的催化作用,目标产物收率为69.1%～94.0%.     

分散液相微萃取-高效液相色谱法测定水中α-萘酚和β-萘酚

以氯苯为萃取剂,丙酮为分散剂,采用分散液相微萃取-液相色谱联用技术对水体中的α-萘酚和β-萘酚进行分析,优化了实验条件。该方法对α-萘酚和β-萘酚的线性范围分别为1.5～50μg/L和1.0～50μg/L,检出限分别为0.9μg/L和0.5μg/L,6次重复测定的相对标准偏差分别为3.3%和1.5%。方法应用于自来水、地下水和湖水样品的分析测定,回收率在91.3%～101.0%之间。     

应用平行因子分析和三维荧光分析法分辨萘、1-萘酚和2-萘酚

首次利用三维荧光分析法与RARAFAC算法相结合,在激发波长为220-300nm2(2nm为间隔）,发射波长为325-600nm(5nm为间隔）对萘、1-萘酚和2-萘酚体系进行了分辨研究,分辨结果与真实结果一致。该方法分辨速度快,易于编程实现,且分辨率高,解决了三者同时分辨难的问题,充分地说明了化学计量学在环境化学中具有广阔的应用前景。     

1-Naphthol as an excited state proton transfer fluorescent probe for sensing bound-water hydration of polyvinyl alcohol

When 1-naphthol incorporated polyvinyl alcohol (PVA) films are allowed to swell in water, there is a loss of fluorescence intensity of the neutral form with a concomitant increase of the anionic form fluorescence intensity. This fluorescence response due to the excited state prototropism (ESPT) of 1-naphthol is very sensitive to the initial stage of hydration of the PVA. Using an existing model of hydrogel swelling and DSC experiments, it was reasoned that 1-naphthol senses the bound-water component of PVA hydration. Thus, 1-naphthol is proposed as an ESPT fluorescent sensor for the specific sensing of bound-water hydration of PVA hydrogel.     

Sorption-Photometric Determination of 1-Naphthol with Polyurethane Foams

Abstract

Two approaches to sorption-photometric determination of 1-naphthol in waters with application of polyurethane foams are offered. The first approach was based on sorption of a coloured 1-naphthol azoderivative, which was formed by the reaction with 4-nitrophenyldiazonium tetrafluoroborate (NFD). In the second variant, 1-naphthol is first sorbed by a polyurethane foam, and it is then transformed into a coloured azoderivative by sorbent treatment of a NFD solution. A coloured 1-naphthol azoderivative was determined immediately in the polyurethane foam using diffuse reflectance spectroscopy. Calibration graphs are linear in the interval of concentrations of 0.01 - 1 μg/ml. The analytical results indicated that a selective and sensitive analytical procedure could be easily applied to determination of 1-naphthol concentration in waters.     

生物膜电极法降解水中2-萘酚的影响因素

以2-萘酚为目标污染物,在对比电化学法和微生物法降解效果的基础上,研究了隔膜式电解体系中基体材料性质、电解池隔膜种类、温度和电流密度对生物膜电极法降解2-萘酚作用效率的影响.结果表明,生物膜电极法相比传统的电化学法和微生物法对2-萘酚类污染物的去除有一定优势,其作用效果与微生物生长状态有直接关系.以碳毡为基体的生物膜电极降解效果起始阶段优于钛网基生物膜电极,但一段时间后钛网基生物膜电极降解性能更稳定.阴离子交换隔膜电解池体系对2-萘酚的降解效果优于阳离子交换隔膜电解池体系,35℃条件下0.5 mA/cm²电流密度是最佳作用条件.     

Spectrofluorimetric Determination of 2-Naphthol in A Pharmaceutical Shampoo Using Anionic SDS Micellar Media

Abstract

Fluorescent characteristics of 2-naphthol were studied in aqueous solution and in micellar solutions of sodium dodecyl sulfate (SDS), hexadecyl-trimethylammonium bromide (HDTB), and Triton X-100. The enhancement of 2-naphthol fluorescence in SDS neutral solutions was used to establish a method for the determination of 2-naphthol. The method was applied in a medicinal shampoo.     

ADSORPTION OF LATERALLY INTERACTING 1-NAPHTHOL/1-NAPHTHYL-AMINE MIXTURES ON NONPOLAR SURFACES FROM AQUEOUS SOLUTIONS

The binary adsorption behavior of 1-naphthol/1-naphthylamine mixtures in water on nonpolar adsorbent Amberlite XAD4 was investigated at 293 K,303 K and 313 K,respectively.The experimental uptakes of 1-naphthol and l-naphthylamine in all binary-component systems of different molar ratios were obviously higher than the corresponding uptakes predicted by the extended Langmuir model,assuming no interaction between the adsorbed molecules of the two components.This phenomenon was attributed to the cooperative adsorption effect arising from the hydrogen bonding interaction between l-naphthol and l-napbthylamine molecules.A modified extended Langmuir model was proposed to describe the binary adsorption behavior by means of introducing a fitting parameter related with the cooperative adsorption effect of the adsorbates.     

Kinetic and Spectroscopic Characterization of 1-Naphthol 2-hydroxylase from Pseudomonas sp. Strain C5

1-Naphthol 2-hydroxylase (1-NH) catalyzes the conversion of 1-naphthol to 1,2-dihydroxynaphthalene. 1-NH from carbaryl degrading Pseudomonas strain C5 was purified and characterized for its kinetic and spectroscopic properties. The enzyme was found to be NAD(P)H-dependent external flavin monooxygenase. Though the kinetic parameters of 1-NH from strain C5 appear to be similar to 1-NH enzyme from strains C4 and C6, however, they differ in their N-terminal sequences, mole content of flavin adenine dinucleotide (FAD), reconstitution of apoenzyme, and K _i. 1-NH showed narrow substrate specificity with comparable hydroxylation efficiency on 1-naphthol and 5-amino 1-naphthol (~30 %) followed by 4-chloro 1-naphthol (~9 %). Salicylate was found to be the nonsubstrate effector. The flavin fluorescence of 1-NH was found to increase in the presence of 1-naphthol (K _d?=?11.3 μM) and salicylate (K _d?=?1027 μM). The circular dichroism (CD) spectra showed significant perturbations in the presence of NAD(P)H, whereas no changes were observed in the presence of 1-naphthol. Naphthalene, 1-chloronaphthalene, 2-napthol, and 2-naphthoic acid were found to be the mixed inhibitors. Chemical modification studies showed the probable involvement of His, Cys, and Tyr in the binding of 1-naphthol, whereas Trp was found to be involved in the binding of NAD(P)H.     

Determination of bisphenol A and naphthols in river water samples by capillary zone electrophoresis after cloud point extraction

As a first attempt, cloud point extraction (CPE) was developed to preconcentrate bisphenol A (BPA), α-naphthol and β-naphthol prior to performing capillary zone electrophoresis (CZE) analysis. The parameters influencing the CPE efficiency, such as Triton X-114 concentrations, pH value, extraction time and temperature were systematically evaluated.After diluting with acetonitrile, the surfactant-rich phase of CPE can be injected directly into the CE instrument. The CZE baseline separation was achieved with running buffer (pH 9.5) composed of 50 mM sodium tetraborate in 30% (v/v) methanol, and an applied voltage of 25 kV. Under the optimized CPE and CZE conditions, an preconcentration factor of 50 times could be obtained and the limit of quantification for the three analytes were found to be 1.67 μg L⁻¹, 0.80 μg L⁻¹ and 0.67 μg L⁻¹ for BPA, α-naphthol and β-naphthol, respectively. The proposed methods have shown to be a green, rapid and effective approach for determination of three analytes present in river water samples.     

1-Naphthol as an excited state proton transfer fluorescent probe for erythrocyte membranes

The microenvironmental dependence of excited state prototropism of 1-naphthol and the corresponding changes in its fluorescence emission is utilized to monitor the acyl chain melting phase transition behavior of liposome membrane made from human erythrocyte lipids. A sharp increase in the ratio of neutral/anionic form fluorescence intensity is noticed at the phase transition temperature (19 degrees C). This provides a convenient method for obtaining phase transition temperature in lipid membranes. The membrane modifying effect of cholesterol on the erythrocyte liposome is successfully sensed by 1-naphthol fluorescence.     

Using an Electrochemical MIP Sensor for Selective Determination of 1-Naphthol in Oilfield Produced Water

A molecularly imprinted polymer (MIP) sensor was successfully constructed on glassy carbon electrode for the determination of 1-naphthol (1-Nph). The sensor was constructed by electropolymerization on bare GCE in the presence of the target molecule. The recognition of 1-Nph was conducted indirectly using [Fe(CN)₆]^3−/4− as redox probe. The MIP sensor presented wide linear working range and limit of detection of 1.5×10⁻⁹ mol L⁻¹. The MIP sensor was applied for the determination of 1-Nph in oilfield produced water. The results obtained showed good selectivity and sensitivity of the proposed sensor in terms of 1-Nph quantification.