Determination of proteins at nanogram levels by a resonance light-scattering technique with tetra-substituted sulphonated aluminum phthalocyanine

This is the first report on the determination of proteins with tetra-substituted sulphonated aluminum phthalocyanine (AlS₄Pc) by resonance light-scattering (RLS). At pH 3.0, the weak RLS of AlS₄Pc can be enhanced by the addition of proteins. Based on this, a novel quantitative method has been developed for the determination of proteins in aqueous solutions. Under optimal conditions, the linear ranges of the calibration curves were 0.050–2.0 μg ml⁻¹ for both human serum albumin (HSA) and human r-IgG. The detection limits were 12.7 ng ml⁻¹ for HSA and 16.1 ng ml⁻¹ for human r-IgG. The method has been applied to the analysis of total protein in human serum samples collected from the hospital and the results were in good agreement with those reported by the hospital, which indicates that the method presented here is not only sensitive, simple, but also reliable and suitable for practical applications.     

Determination of lithium in human serum by electrothermal atomic absorption spectrometry

An efficient method was developed for the determination of nanogram levels of lithium in biological samples. Serum samples from human subjects from southeastern Spain, treated or not treated with lithium carbonate, were analyzed by electrothermal atomic absorption spectrometry. The samples were previously treated with a matrix modifier consisting of 0.1% Triton X-100 and injected through a graphite tube with L'vov platform. The Li concentrations measured by the procedure described for the 3 certified reference samples used were not significantly different (p > 0.05) than certified levels. Sample recoveries and variability during several days, with coefficients of variation from 4.00 to 14.8%, demonstrated the reliability and accuracy of this technique. Mean Li concentration determined in the serum of individuals with psychiatric disorders treated with Li (n = 117, 5.077 +/- 1.795 microg Li/mL) was significantly higher (p < 0.001) than that in individuals not treated with Li (n = 24, 1.902 +/- 2.054 ng Li/mL).     

Development and validation of a high-performance liquid chromatographic method using fluorimetric detection for the determination of the diarrhetic shellfish poisoning toxin okadaic acid without chlorinated solvents

A modification of the high-performance liquid chromatographic method with fluorimetric detection method for the determination of diarrhetic shellfish poisoning toxins was developed to completely avoid the use of dangerous chlorinated solvents. The method was validated for the toxin okadaic acid (OA) over a period of 6 months where 12 calibrations were performed and 72 samples were analyzed. Analysis of toxic and non-toxic mussels, clams and scallops demonstrated its selectivity. Linearity was observed in the tested range of interest for monitoring purposes of edible shellfish, from the limit of detection (0.3 microg OA/g hepatopancreas) to 13 microg OA/g hepatopancreas. Intra-assay precision of the method was 7% RSD at the quantification limit (0.97 microg OA/g hepatopancreas at S/N=10). Accuracy was tested in triplicate recovery experiments from OA-spiked shellfish where recovery ranged from 92 to 106% in the concentration range of 0.8 to 3.6 microg OA/g hepatopancreas. Useful information on critical factors affecting calibration and reproducibility is also reported. Good correlation (R=0.87) was observed between the results of the method and those of the method of Lee, after the analysis of 45 samples of mussels from the galician rias.     

Thermal Behaviour and Decomposition Kinetics for Two Palladium(II) Complexes with 1-aminopyrene and its Derivative

The thermal decomposition studies for two palladium(II) complexes Pd(apyr)₂Cl₂ and Pd(pmpa)Cl₂ (apyr=1–aminopyrene and pmpa=N–(2–pyridylmethylene)–1–pyrenylamine) were carried out in pure nitrogen using TG-DTG techniques. The non-isothermal kinetic parameters for the two complexes were evaluated employing the method suggested by Málek, esták, Koga et al. Based on the above results, thermal behaviour of the complexes were carefully discussed, which showed that not only the parameters value, but also the decomposition pattern and mechanism for complex 1 are different from complex 2.This revised version was published online in November 2005 with corrections to the Cover Date.     

Determination of 20-hydroxyecdysone content by thin-layer chromatography and micellar electrokinetic chromatography

Summary Seasonal dependence of 20-hydroxyecdysone content ofSerratula tinctoria andSerratula wolffii (Asteraceae) was investigated by micellar electrokinetic chromatography (MEKC). Samples were collected each month through the vegetation period. The leaves were dried, milled and extracted with methanol. Clean-up of the extracts was by solid-phase extraction using a polyamide micro-column to remove flavonoids and other plant phenolics which can interfere with the analysis. This work deals with the separation of 20-hydroxyecdysone from polypodine B and the seasonal variation of 20-hydroxyecdysone concentration. Determinations have been performed by both thin-layer chromatography and capillary electrophoresis using micellar electrokinetic chromatography. Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997.     

Syntheses and Structural Aspects of Cyclodextrin/Dialkylamine Inclusion Compounds

We report the syntheses and structural aspects of cyclodextrin host–guest inclusion compounds containing linear secondary alkylamines (dipropyl, dibutyl, dipentyl, dihexyl, and dioctyl) at 25 °C. Elemental analysis, ¹³C CP-MAS NMR spectroscopy, and powder X-ray diffraction analysis confirm the inclusion process. The basic host structure of the products is similar to that of typical cyclodextrin inclusion systems. ¹³C MAS NMR experiments show a different resonance pattern for the confined guest molecules with respect to the amine in the liquid phase. The presence of different resonance signals for the homologous carbon atoms of both dialkylamine branches is evidence for the non-symmetric location of the amine in the cyclodextrin channels.     

Synthesis and properties of novel dialkylaminocarbenium salts

Novel dialkylaminocarbenium salts with metallocomplex counter ions were prepared by the reaction of phosgene with either DMF or tetramethylurea in the presence of metal chlorides. Reactions of organosilicon amides with phosgene gave corresponding carbenium salts, while organosilicon ureas yielded aminoiminocarbenium salts. Dialkylaminochlorocarbenium salts were reduced with hydrosilanes to give dialkylaminocarbenium, salts and can be easily hydrolyzed to afford either amides or ureas. Pathways of the reaction with water and alcohols depend on the nature of reagent and the reaction conditions. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 1035–1040, May 1997.     

Bradykinin-potentiating peptide from venom of the spider Latrodectus tredecimguttatus

A bradykinin-potentiating peptide has been isolated from the venom of the spiderLatrodectus tredecimguttatus. Its physicochemical properties and amino acid composition have been investigated in detail. It has been shown by biological testing on isolated neck of the rat uterus that the peptide increases the contractile effect of bradykinin in in vitro experiments. The “potentiating unit” is 2 · 10^?3 mg/ml. A 50% increase in the hypotensive effect of bradykinin at a concentration of the bradykinin-potentiating peptide of 15 µg/kg of body weight has been found, the increase in the intensity of the effect being accompanied by a prolongation of its action.     

Estimation and prediction of the retention indices of selectedtrans-diazenes

Chromatographia - The gas chromatographic retention indices of some typicaltrans-diazenes were determined on a methyl silicone capillary column. Thetrans-diazenes are less strongly retained than...     

Reaction gas chromatography: Study of the photodecomposition of selected substances

Summary A simple apparatus that permits to carry out photolytic reactions in direct connection with a gas chromatograph has been designed. The photodecomposition of C₅–C₇ aliphatic alkanes, C₁–C₅ primary, secondary and tertiary aliphatic alcohols and of some other substances was studied using this apparatus. The degradation products are characteristic of the individual types of alcohols. The identification of the individual types of alcohols. The identification of the degradation products confirms the proposed schemes for the photodegradation reactions. The apparatus described can also be used for the study of photolysis kinetics, as it permits the easy and rapid variation of the reaction conditions.