琥乙红霉素与紫色素的荷移反应及其测定

建立了一种快速测定琥乙红霉素的荷移分光光度法。琥乙红霉素与紫色素在乙醇-水介质中发生电荷转移反应,荷移络合物在546 nm波长处有最大吸收,表观摩尔吸光系数为9.18×103L.mol-1.cm-1,络合物的组成为1∶1,稳定常数为1.9×105。药物质量浓度在0~90 mg.L-1范围内服从比耳定律,相关系数为0.999 7,当琥乙红霉素质量浓度为40 mg.L-1时,6次测定结果的相对标准偏差为1.24%。测定了琥乙红霉素片剂中有效成分的含量,并与药典方法进行比较,结果基本吻合。     

Development and Evaluation of a Kinetic‐Spectrophotometric Method for Determination of Arginine

A kinetic method for the determination of micro quantities of amino acid arginine (Arg) is described in this paper. The catalytic activity of cobalt in the reaction of oxidation of purpurin (1,2,4‐trihydroxy‐antraquinone, PP) by hydrogen peroxide in alkaline buffer solution decreases in the presence of micro quantities of arginine, because of the formation of the complex. Operating conditions for the successful determination of arginine were optimized. The optimized conditions yielded a theoretical detection limit of 1.45 μg mL^?1. Kinetic equations are proposed for the investigated process. The interference effects of certain foreign ions and amino acids upon the reaction rate were studied and removed in order to assess the selectivity of the method. The developed procedure was successfully applied to the determination of arginine in various pharmaceutical samples. The typical feature of this procedure is that determination can be carried out at room temperature and in a short analysis time. The newly developed method is simple, inexpensive and efficient for use in the analysis of a large number of samples.     

H‐Point Standard Addition Method Applied to Voltammetry of Microparticles. Quantitation of Dyes in Pictorial Samples

A solid‐state electrochemical application of the H‐point standard addition method (HPSAM) for quantifying two electroactive compounds, A, B, that produce strongly overlapped voltammetric peaks is described. It is based on peak current measurement in square‐wave voltammograms recorded for solid samples containing a reference compound R, upon additions of a A‐ (or B‐) containing standard compound. The method allows to the determination of the mass fraction of A and B by applying the H‐point standard addition method to solid state voltammetry. The quotients between the currents measured at two selected potentials and the peak current of R vary linearly with the mass ratio of the added standard and the reference compound, thus providing an electrochemical method for determining the content of A and B in the sample avoiding matrix effects. The method is applied to the simultaneous determination of alizarin and purpurin in madder pigments and pictorial specimens using morin as a reference material.     

交沙霉素与红紫素的荷移反应及其测定

交沙霉素与红紫素在乙醇-水介质中发生电荷转移反应,荷移络合物在545nm处有最大吸收,表观摩尔吸光系数是4.09×103L·mol-1·cm-1,该络合物的组成是1∶1,稳定常数是3.9×104.药物浓度在0-120mg/L范围内服从比耳定律,建立了一种测定交沙霉素的荷移分光光度法.当交沙霉素浓度为80mg/L时,6次测定结果的相对标准偏差为1.84%.利用本法测定了交沙霉素制剂中有效成分的含量,并与文献法进行比较,二者结果基本吻合,回收率在96%以上.     

A spectrometric and chromatographic approach to the study of ageing of madder (Rubia tinctorum L.) dyestuff on wool

In this work, the lightfastness of wool textile samples, dyed with madder and its principal components alizarin and purpurin, was investigated using two complementary experimental techniques: absorption and emission UV-vis spectroscopy and chromatography (HPLC-PDA). Spectroscopic techniques were used to follow the time course of ageing, whereas chromatography was applied to determine relative compositional changes that occurred after exposure of wool dyed samples to natural and artificial ageing. The results from the two techniques integrate well each other and provide complementary and useful indications about the sensitivity of the dyed textiles to ageing, showing that purpurin is the principal component responsible for the spectral and chromatic properties of madder as well as for its degradation. The fading of both the fibre and dye is reduced in the presence of alum and in the absence of oxygen. The multi-analytical approach used highlights the potential of the UV-vis spectroscopy for the investigation of dyes on textiles. The great sensitivity of the spectrofluorimetry makes this technique particularly promising for a non-destructive study of dyes on works of art.     

Optimization of microwave-assisted extraction for alizarin and purpurin in Rubiaceae plants and its comparison with conventional extraction methods

A simple and rapid microwave-assisted extraction (MAE) procedure was developed and optimized for two common color pigments, alizarin and purpurin, in various samples of Rubiaceae plants. Several variables that can potentially affect the extraction efficiency, namely temperature, methanol concentration in the extractant mixture, time, and solvent volume were optimized by means of a central composite design approach. The results suggest that temperature and methanol concentration in the solvent mixture are statistically the most significant factors. The separation and quantitative determination of the pigments was carried out in less than 6 min by a developed high-performance liquid chromatographic method with UV detection at 250 nm. Under optimum operating conditions, MAE showed significantly higher recoveries than those obtained by the conventional extraction methods (ultrasonic and reflux extraction), ranging from 84 to 94%. In addition, a drastic reduction of the extraction time (20 min versus 6 h) and solvent consumption (20 versus 100 mL) was achieved with a reproducibility (RSDs < 10%) comparable with that provided by the reflux extraction as a reference method.     

荷移分光光度法测定酒石酸美托洛尔

研究了酒石酸美托洛尔与紫色素之间的荷移反应。确定了反应条件,建立了一种测定酒石酸美托洛尔的荷移分光光度法。酒石酸美托洛尔与紫色素在乙醇介质中,室温条件下即可形成稳定的1∶1型荷移络合物,该络合物的最大吸收波长为540 nm,表观摩尔吸光率为6.83×103L.mol-1.cm-1。酒石酸美托洛尔质量浓度在10~80 mg/L范围内服从比耳定律,相关系数为0.9991。相对标准偏差为1.3%(n=11),回收率为99.3%~102.7%。     

荷移分光光度法测定醋酸氯己定

通过醋酸氯己定与红紫素的荷移反应来测定制剂中醋酸氯己定的含量,是利用分光光度法进行测定的。反应在乙醇-丙酮介质中进行,反应物的最大吸收波长为545 mn,表观摩尔吸光系数为1.54×10~4 L·mol-1·cm-1,相对标准偏差为0.89％(n=6),药物浓度在0-45 mg·L-1范围内呈线性关系;此方法简便易行,条件易于控制,灵敏度高,对样品的测定结果令人满意。     

Artificial photosynthetic reaction centers with carotenoid antennas

Two reaction center-antenna models based on a purpurin macrocycle linked to a C₆₀ and to a carotenoid polyene have been synthesized. In these systems the C₆₀ moiety is the primary electron acceptor, the purpurin is the primary electron donor and the carotenoid moiety acts both as an antenna and secondary electron donor. Formation of the initial charge separated state, C-Pur⁺-C₆₀⁻, following excitation with light absorbed by either the purpurin or C₆₀ takes place on the 10 ps time scale. The final charge separated state, C⁺-Pur-C₆₀⁻, is formed in one of the compounds with a quantum yield of 32% based upon light absorbed by the carotenoid. In order to function as an antenna, the carotenoid pigment must be electronically coupled to the purpurin. The purpurin C ring provides an excellent framework for locating a carotenoid polyene in partial conjugation with the macrocycle, leading to a relatively strong electronic communication between the chromophores; functionalization of a meso position of the purpurin provides a site for the covalent attachment of C₆₀.     

Organotin Complexes of Alizarin and Purpurin

Five novel organotin complexes with the anthraquinone dyes alizarin (1,2‐dihydroxyanthraquinone) and purpurin (1,2,4‐trihydroxyanthraquinone) were synthesized and characterized by elemental analyses, FTIR and NMR spectroscopy (¹H, ¹³C and ¹¹⁹Sn). The crystal and molecular structures of four complexes were determined by X‐ray diffraction on single crystals: [Bu₂Sn(aliz)(H₂O)]·C₂H₅OH ( A1 ·EtOH), [Bu₂Sn(aliz)(dmso)]₂ ( A3 ), [(Bu₂Sn)₃O(Hpurp)₂] ( P1 ) and [Bu₂Sn(Hpurp)(dmso)]₂ ( P2 ), where H₂aliz = alizarin and H₃purp = purpurin. The coordination mode of the ligands is identical to that found in their Al/Ca complexes, where they act as dianionic tridentate ligands forming five and six‐membered fused chelate rings. The coordination to the tin atoms occurs exclusively via the 1,2‐ phenolate oxygen and the adjacent quinoid oxygen atoms. The complexes A1 , A3 and P1 are dimers with hepta‐coordinated tin atoms in form of a slightly distorted pentagonal bipyramid. The trinuclear complex P2 contains two pentacoordinated and one heptacoordinated tin atoms.