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151.
吴庆生  程丽娅 《分析化学》1995,23(11):1337-1340
本采用压缩X因子导数光谱技术实现了宽峰体系灵敏度的大幅度提高,提出了测定痕量锗的方法。在0.72mol/LH2SO4和3.0mol/LH3PO4的混酸介质中,锗-水杨基荧光酮-OP三元显色体系的压缩X因子四阶导数光谱摩尔响应系数达1.89×10^6L.mol^-1.cm^-1,灵敏度比常规光度法高12.4倍;最低检测出限为0.00033mg/L,比常规光谱法低4倍;选择性也进一步提高,绝大多数离  相似文献   
152.
在酸性介质中,偶氮胭脂红B(ABX)与蛋白质在室温下能迅速结合生成复合物,其最大吸收波长为570nm,比ABX红移了50nm。本文用光度法研究了该结合反应的最佳条件,并在此基础上建立了一个测定蛋白质的新方法。在570nm处各蛋白质的浓度至少在2.5~120mg/L范围内与吸光度成正比,对测定牛血清蛋白质(BSA)、人血清蛋白(HSA)及γ-球蛋白(IgG)的桑德尔灵敏度分别为0.173、0.173和0.199μg/cm^2。除阴阳离子表面活性剂外,基余大部分物质不干扰蛋白质的测定。可见方法具有选择性好、灵敏度高且快速、稳定的优点,用于尿液及人血清样品中总蛋白的测定,所得结果与考马斯亮蓝方法测得结果基本一致。  相似文献   
153.
A detection scheme for the simultaneous evaluation of two bioassays based on fluorescence spectroscopy is presented. For the determination of hydrogen peroxide-generating enzymes or peroxidases, the non-fluorescent 4-(N-methylhydrazino)-7-nitro-2,1,3-benzooxadiazole (MNBDH) is converted to the strongly fluorescent 4-(N-methylamino)-7-nitro-2,1,3-benzooxadiazole (MNBDA). Phosphatases are detected based on the cleavage of the non-fluorescent 5-fluorosalicyl phosphate (5-FSAP) under formation of the fluorescent 5-fluorosalicylic acid (5-FSA). While excitation of the fluorophores may be carried out at the same wavelength, their emission spectra differ significantly. This allows the read-out of both assays using commercially available microplate readers without additional chemometric tools. Compared with individual assays, limits of detection are similar, and linearity of the calibration functions for both enzymes is observed over 2-3 concentration decades starting at the limit of quantification. The simultaneous determination of glucose oxidase and acid phosphatase in honey is presented as example for the application of the detection scheme.  相似文献   
154.
Three highly sensitive spectrophotometric methods for the determination of platinum(IV) have been developed, based on its colour reactions with molybdate and basic dyes (BD) in aqueous solution in the presence of poly(vinyl alcohol). Platinum(IV) reacts with molybdate and BD to form ion — association complexes of composition (BD)2[Pt (MoO4)3]. The molar absorptivities are between 6.83 × 105 and 9.51 × 105 dm3mol–1cm–1, the highest value being found with nile blue. Suitable conditions for the reactions and the effects of foreign ions were investigated. The methods can be applied to the spectrophotometric determination of trace amounts of platinum(IV) in some catalysts and ores.  相似文献   
155.
Multicommutation implemented with flow-through optosensors is a very promising area of research. This recent approach benefits from the advantages of both methods and results in high sensitivity, selectivity, and speed, and little waste generation. This paper reports the simultaneous determination of furosemide and triamterene, two widely used diuretics, by measurement of their native fluorescence. The system has been proved to be useful for determination of both analytes in pharmaceutical preparations and for determination of triamterene in human urine and serum. A minicolumn filled with Sephadex SPC-25 microbeads was used to achieve separation of both analytes before detection in a flow-through cell filled with the same resin. The sensor is linear in the range 50–1200 and 0.4–8 ng mL−1 with detection limits of 15 and 0.1 ng mL−1 for furosemide and triamterene, respectively.  相似文献   
156.
利用电荷迁移反应测定头孢羟氨苄   总被引:4,自引:0,他引:4  
陈学诚  容彦华 《分析化学》1998,26(3):310-313
提出一种基于电荷迁移反应简便可靠地测定头孢羟氨苄的分光光度法。在甲醇-乙醇介质中,头孢羟氨苄与氯冉酸于50℃反应15min能够形成稳定的1:1络合物,其λmax=528nm,线性范围为20 ̄400mg/L。用拟定的方法测定原粉和胶囊,结果与药典法一致。对浓度100mg/L的药物10次测定相对标准偏差为1.4%,样品的标准加入回收率为99.0% ̄100.8%。  相似文献   
157.
Summary The 1,6-dioxo-tautomer of hypericin was obtained by basic and BF3 catalyzed tautomerization of the natural and most stable 7,14-dioxo-tautomer. The isolation of this tautomer was aided by its insolubility in methanol. It was identified and characterized by spectroscopic methods, and its detailed structure was derived by means of force field calculations.
Zur Tautomerie des Hypericins: Das 1,6-Dioxo-Tautomere
Zusammenfassung Das 1,6-Dioxo-Tautomere des Hypericins wurde durch basen- und BF3-katalysierte Tautomerisierung des natürlichen, stabilen 7,14-Dioxo-Tautomers erhalten. Dessen Isolierung wurde durch die Schwerlöslichkeit in Methanol ermöglicht. Es wurde durch spektroskopische Methoden identifiziert und charakterisiert, und seine detaillierte Struktur wurde aus Kraftfeld-Rechnungen abgeleitet.
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158.
The UV-vis absorption and the fluorescence emission spectra of novocaine were analysed in aqueous cyclodextrin (CD) solutions. Either the absorbance read at λmax 290 nm or the fluorescence emission intensity at λems 346 nm increase in the presence of both α- and β-CD due to the formation of 1:1 inclusion complexes. The lower polarity of the CD-cavity sensed by the included drug enhances the emitted fluorescence; in fact, the same effect was observed in aqueous mixtures of acetonitrile, dioxane, or dimethylsulfoxide. The inclusion complex formation between the monocation of novocaine and CDs diminishes the electrical conductance of aqueous solutions of novocaine hydrochloride (NoHCl). Both the nitrosation reaction in aqueous acid medium and the ester hydrolysis in alkaline medium are retarded in the presence of CDs. The strongest effect was observed with β-CD as a consequence of the higher stability inclusion complex.  相似文献   
159.
The formation of charge transfer complexes with 1:1 and 2:1 stoichiometries (acceptor-to-donor) between DDQ and 1,10-diaza-18-crown-6 in chloroform solution was investigated spectrophotometrically. The stepwise formation constants of the resulting complexes were evaluated from the non-linear least-squaresfitting of the absorbance-mole ratio data. The enthalpies and entropiesof the complexation reactions were determined from the temperature dependence of the stepwise formation constants. The resulting 1:1 and 2:1 complexes were isolated in crystalline form and characterized. The results are consistent with the ionic structure of the resulting charge transfer complexes.  相似文献   
160.
Summary Stepwise electrophilic bromination of hypericin in pyridine as the solvent yields regioselectively 2,5-dibromohypericin, 2,5,9-tribromohypericin, and 2,5,9,12-tetrabromohypericin. The compounds were characterized by means of NMR-, UV-Vis-, and fluorescence-spectra, andpK a andpK* a measurements. These properties were compared with those of hypericin on the one hand and of the recently isolated gymnochromes on the other hand.
Zur Bromierung des Hypericins: Die Gymnochrom-Chromophore
Zusammenfassung Schrittweise elektrophile Bromierung von Hypericin in Pyridin als Lösungsmittel liefert regioselektiv 2,5-Dibromhypericin, 2,5,9-Tribromhypericin und 2,5,9,12-Tetrabromhypericin. Diese Verbindungen wurden durch NMR-, UV-Vis- und Fluoreszenz-Spektrometrie sowie durchpK a - undpk* a -Messungen charakterisiert. Diese Eigenschaften wurden mit jenen des Hypericins und der kürzlich isolierten Gymnochrome verglichen.
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