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Showing papers on "Reagent published in 1977"


Journal ArticleDOI
TL;DR: Although many of the C-3 substituted indoles such as indole-3-acetic acid and tryptamine had colors in the reddish-violet-blue color region, most exhibited sufficient color differentiation to allow their identification by thin-layer chromatography.

341 citations


Journal ArticleDOI
TL;DR: The rate constants for thiol-disulfide interchange between 21 mono- and dithiols and Ellman's reagent correlate with the pKu's of the thiol groups with a Bronsted coefficient of p = 0.36, and a convenient synthesis of a mixture of diastereomers of 1,4-dimercapto-2,3-butanediol has been developed.
Abstract: The rate constants for thiol-disulfide interchange between 21 mono- and dithiols and Ellman's reagent correlate with the pKu's of the thiol groups with a Bronsted coefficient of p = 0.36. The maximum rates ofreduction are observed for thiols having pK, values close to the pH of the solution in which the reactions were carried out. In the dilute solutions examined (10-4-10-6 M in each reagent), the rate of the second, intramolecular interchange step in reactions of dithiols was faster than that of the first, intermolecular interchange, regardless of the size of the cyclic disulfide formed. A convenient synthesis of a mixture of diastereomers of 1,4-dimercapto-2,3-butanediol (i.e., of a mixture of dithiothreitol, DTT, and dithioerythritol, DTE) has been developed from 1,2:,4-diepoxybutane and thiolacetic acid.

215 citations



Journal ArticleDOI
TL;DR: Addition of sodium bismuth tartrate to a carbohydrate reagent consisting of 4-hydroxybenzoic acid hydrazide in aqueous sodium hydroxide enables the reaction to be carried out more rapidly, at a lower temperature, and with four- to fivefold greater sensitivity.

191 citations



Journal ArticleDOI
TL;DR: A survey of the reaction of carbodiimide alone with eleven typical proteins indicates that the reagent itself may be suitable for selective modification of only a few residues, including carboxylic acid side chains partially buried on the surface or in active sites.

148 citations


Journal ArticleDOI
01 Jan 1977-Analyst
TL;DR: In this article, the turbidimetric determination of sulphate as barium sulphate has been adapted to the continuous flow injection procedure of Růžicka and co-workers.
Abstract: The turbidimetric determination of sulphate as barium sulphate has been adapted to the continuous flow injection procedure of Růžicka and co-workers. The effects of reagent composition, reagent flow-rates and length of mixing coils have been investigated. Optimum conditions were established for the determination of sulphate in natural waters and in plant digests. The results agree satisfactorily with those obtained by a standard turbidimetric method and analyses can be carried out at a rate of up to 180 samples per hour.

132 citations


Journal ArticleDOI
TL;DR: The method appears especially suitable for adaptation to discrete mechanical analyzers either of the single channel or the multi-channel type, and can be lowered by a factor of 2.2 by replacing phenol by dihalogen phenols.
Abstract: A fully enzymatic method to determine total cholesterol in serum is described. The method appears especially suitable for adaptation to discrete mechanical analyzers either of the single channel or the multi-channel type. The method uses the enzymes cholesterol esterase (EC 3.1.1.13), cholesterol oxidase (EC 1.1.3.6) and peroxidase (EC 1.11.1.7) with 4-aminophenazone and phenol as substrates in the indicator reaction. The method was adapted to the Greiner Selective Analyzer GSA-II. For this purpose the critical parameters of the reaction were intensively examined. The complete reagent is stable within the GSA II dispenser at 4 degrees C for at least 1 week. By omitting cholesterol oxidase in the blank reagent a sample bland and a partial reagent blank are obtained. Within a range up to 10.4 mmol/1 (4.0 g/l) the maximum colour is developed within 6 minutes. The calibration factor was stable for 4 months. The method allows absolute measurements. At concentrations between 2 and 4 mmol/1 within-batch precision ranged from 0.5 to 1.4%. Precision from day to day for the same control sera amounted to 2.8; 2.0; 2.7 and 2.0% for a period of 3 months. Examination of accuracy yielded satisfying results. Ascorbic acid in the physiological range did not alter results to a significant extent. Catalase or novaminesulfone added in vitro did not interfere. Optical interferences by bilirubin, hemoglobin or turbidity are compensated by a sample blank. A comparison of results with the enzymatic method of Roeschlau et al. (Z. Klin. Chem. Klin. Biochem. 12, 226 (1974)) yielded satisfactory agreement. The limits of detection of the present method can be lowered by a factor of 2.2 by replacing phenol by dihalogen phenols.

127 citations


Patent
01 Aug 1977
TL;DR: In this article, an improved multilayer element for detecting glucose in samples of biological fluid which may contain with fluoride ion as a contaminant or preservative is described, which comprises a buffered Trinder's reagent, which reagent comprises glucose oxidase, peroxidase, 4-aminoantipyrine and a phenolic or naphtholic coupler, which is buffered to a pH between about 4.5 and about 6.
Abstract: An improved multilayer element for detecting glucose in samples of biological fluid which may contain with fluoride ion as a contaminant or preservative is described. The improved element comprises a buffered Trinder's reagent, which reagent comprises glucose oxidase, peroxidase, 4-aminoantipyrine and a phenolic or naphtholic coupler, which is buffered to a pH between about 4.5 and about 6.0. Such a buffering reduces any interference which may be due to fluoride ion present in the sample under analysis.

119 citations


Journal ArticleDOI
TL;DR: In this article, a trajectory study of the exothermic reaction F + H2→ HF + H is presented, where the authors show that an early barrier has the consequence that reagent translation is much more efficient than vibration in promoting reaction even for energies well in excess of the barrier.
Abstract: Concepts developed in recent years as a result of experimental and theoretical studies of the dynamics of reactions A + BC → AB + C are examined here in trajectory studies of the reaction F + H2→ HF + H—currently the prototype of exothermic reaction. (i) An “early” barrier, characteristic of substantially exothermic reaction, has the consequence that reagent translation is much more efficient than vibration in promoting reaction, even for energies well in excess of the barrier. (ii) High vibrational excitation in the molecular product stems from the release of H·H repulsion while the new bond, F––H, is still extended (termed “mixed energy-release”); the large zero point vibration in H2 introduces variability in the F––H extension and H·H repulsion, and consequently in the breadth of the observed product vibrational distribution. (iii) Since the product vibrational excitation is governed by the attractive plus mixed energy-release, the slope of the outrun of the energy surface is not, per se, a dominant factor governing product vibrational excitation. (iv) Enhanced reagent vibration, 〈ΔV〉, tends to be channelled into enhanced product vibration, 〈ΔV′〉; the efficiency (〈ΔV′〉= 0.81 ΔV) is dependent on the form of energy surface in the region of “corner-cutting”, corresponding to reaction through extended intermediates F––H–H. (v) Enhanced reagent translation is channelled into product translation plus rotation (〈ΔT′〉+〈ΔR′〉= 1.12 〈ΔT〉); the efficiency provides an indication of the energy required to bend and compress the intermediate FH·H. (vi) The rotational dependence of the reactive cross section, σ(J), provides a sensitive probe of the region of the potential-energy hyper-surface along the entry valley up to the barrier. (vii) Enhanced reagent rotational excitation at first decreases product vibrational excitation and then increases it according to experiment; this effect has not been reproduced theoretically. (viii) Product rotational excitation derives in large part from the release of repulsion in bent configurations: this gives rise predominantly to coplanarity and opposed directions for the product rotational and orbital motions. (ix) Enhanced reagent excitation of all sorts results in significant enhancement in product rotation, due to reaction through more-compressed and bent configurations; the most efficient conversion is from reagent rotation into product rotation (〈ΔR′〉= 1.2 〈ΔR〉). (x) For thermal (300 K) reaction the computed centre-of-mass angular distribution is sharply backward-peaked, and similar for all product vibrational levels. (xi) Enhanced reagent vibration or translation shifts the computed mean scattering angle forward, with ΔT being markedly more effective than ΔV; the “stripping threshold energy” is high, as anticipated for these masses reacting on a strongly repulsive potential-energy surface favouring collinear approach.

119 citations



Journal ArticleDOI
TL;DR: A new assay for polyols was developed that minimizes interference by sugars based on oxidation of alditols to formaldehyde by acidic periodate, reduction of the excess periodate with l -rhamnose, and a short-time determination of the formaldehyde with the Nash reagent.

Book ChapterDOI
TL;DR: The recent introduction of fluorescamine, a novel reagent designed after the fluorogenic reaction of ninhydrin with primary amines in the presence of phenylalanine, has now provided a strong alternative to ninHydrin for detection of peptides.
Abstract: Publisher Summary The recent introduction of fluorescamine, a novel reagent designed after the fluorogenic reaction of ninhydrin with primary amines in the presence of phenylalanine, has now provided a strong alternative to ninhydrin for detection of peptides Fluorescamine reacts with primary amino groups of peptides almost instantaneously at room temperature in aqueous solution at pH 75-9, to form a fuorescent compound The reagent is subsequently hydrolyzed to yield a watersoluble, nonfluorescent product Fluorescamine itself is not fluorescent Ammonia in solution yields little or no fluorescence with fluorescamine These features and the great sensitivity attainable in the fluorescence measurement have made fiuorescamine increasingly popular in amino acid and peptide analysis Another development in recent years is the rediscovery of o -phthalaldehyde as a general reagent for amino acids and peptides when used in the presence of 2-mercaptoethanol This reagent has recently been applied to the microanalysis of amino acids and peptides

Journal ArticleDOI
TL;DR: A small fraction of the activated lectins were cross-linked to receptors in the membrane upon photolysis and the efficiency of such cross-links of ligands to receptors may be increased by employing longer versions of the hetero-bifunctional cross-linking reagents and also by attaching more of the reagent molecule to ligands.

Journal ArticleDOI
TL;DR: An improved method for the partial chemical synthesis of unsaturated and radioactively labeled phosphatidylcholines is described and sn-glycero-3-phosphorylcholine is reacted with twice the theoretical amount of fatty acid imidazolide and sodium methylsulfinylmethide in dimethylsulfoxide for several minutes at 17 degrees C.

Journal ArticleDOI
TL;DR: In this paper, a new crown ether, 4′-picrylaminobenzo-15-crown-5 (HL), was used for the extraction of alkali metal ions.
Abstract: The extraction study of alkali metal ions was made with a new type of crown ether, 4′-picrylaminobenzo-15-crown-5 (HL). Upon dissociation in alkaline medium orange-colored HL gives blood-red anion, L−, and extracts selectively K+ (and to a lesser extent Rb+) ion into chloroform as a colored complex of composition ML·HL. A colorimetric determination of 10 - 400 ppm K+ in the presence of < 2000 ppm Na+ was possible using this new crown ether reagent.

Journal ArticleDOI
TL;DR: Trialkylzinclithium is readily prepared in THF by mixing zinc chloride (or its TMEDA complex) and alkyllithium in a 1 : 3 mole ratio as mentioned in this paper.
Abstract: Trialkylzinclithium is readily prepared in THF by mixing zinc chloride (or its TMEDA complex) and alkyllithium in a 1 : 3 mole ratio. Conjugate addition of this new reagent is demonstrated with 2-cyclohexen-1-one (I) and dicyclopentadien-1-one (IV) as a,α,β-unsaturated ketones.

Patent
10 May 1977
TL;DR: In this paper, a method and reagent means for the determination of small quantities of chemical compounds in man, animal and plants by a specific binding assay technique is presented. The method involves the utilization of a labelling constituent comprising a conjugate of a labeling substance and a binding component being one or more metal atoms which can be easily determined.
Abstract: A method and reagent means for the determination of small quantities of chemical compounds in man, animal and plants by a specific binding assay technique. The method involves the utilization of a labelling constituent comprising a conjugate of a labelling substance and a binding component said labelling substance being one or more metal atoms which can be easily determined. The labelling constituents are selected from various metalo organic derivatives or metal coordination complexes. The method is very specific and sensitive and can be successfully utilized for the determination of haptens selected from various groups such as alkaloids, barbiturates, steroids, cannabinoids, vitamins, aminoacids, tranquilizers, sugars, penicillins, etc.

Journal ArticleDOI
Gad Avigad1
TL;DR: Reducing sugars, particularly aldoses, react readily with dansyl hydrazine and the fluorescent hydrazones produced can be separated by thin-layer chromatography and determined quantitatively by spectrofluorimetry after elution from the chromatograms.

Journal ArticleDOI
TL;DR: Girard-T reagent (trimethylaminoacetohydrazide chloride) under mild acid or alkaline conditions, reacts with aldehydes and ketones containing α-dicarbonyl functional groups to produce addition compounds which strongly absorb ultraviolet light.

Journal ArticleDOI
TL;DR: Proteins exposed on the outer surface of the outer membrane of Salmonella typhimurium were identified by reacting intact cells with a covalent labeling reagent, and showed that out of the four "major" proteins, three were exposed, and that at least six other proteins were also exposed on cell surface.

Patent
09 Jun 1977
TL;DR: An analytical element for use in the clinical assay of an analyte contained in a biological liquid sample which is applied from an external source to a substantially planar sample receiving suface of the element is described in this article.
Abstract: An analytical element for use in the clinical assay of an analyte contained in a biological liquid sample which is applied from an external source to a substantially planar sample receiving suface of the element. The analytical element comprises a porous layer bearing the aforementioned sample receiving surface; at least one dry reagent material for use in the assay; and one or more associated rupturable pod-like member(s) containing a liquid reagent for the assay, such liquid reagent, upon rupture of the pod-like member(s), being released into the element.

Journal ArticleDOI
TL;DR: The well known air segmentation principle used in connection with Auto-Analyzers was applied successfully to members of the C-group of cardiac glycosides, which were separated on a reversed phase HPLC system and the improvement in the detection limit was at least 100-fold in comparison with UV detection.



Patent
11 Feb 1977
TL;DR: An assay kit for assaying adenosine-3,5'-cyclic monophosphate, which is referred to as cAMP, guanosine and cGMP, or both, is described in this article.
Abstract: An assay kit for assaying adenosine-3',5'-cyclic monophosphate, which is herein referred to as cAMP, guanosine-3',5'-cyclic monophosphate, which is herein referred to as a cGMP, or both; and said assay kit comprising, A container of Reagent 1 comprising succinyl cAMP tyrosine methyl ester; succinyl cGMP tyrosine methyl ester; succinyl cAMP tyrosine methyl ester and succinyl cGMP tyrosine methyl ester in admixture or both succinyl cAMP tyrosine methyl ester and succinyl cGMP tyrosine methyl ester in separate containers, said esters labelled with radioactive iodine; A container of Reagent 2 comprising an anti-cAMP serum, an anti-cGMP serum, an anti-cAMP and anti-cGMP serum in admixture or both anti-cAMP serum and anti-cGMP serum in separate containers; A container of Reagent 3 comprising an imidazole buffer solution of 0.1 M or higher concentration; A container of Reagent 4 comprising a material for separation; A container of Reagent 5 comprising a solution of succinic anhydride in an organic solvent; A container of Reagent 6 comprising an organic tertiary amine; and A container of Reagent 7 comprising a standard solution of cAMP, cGMP, cAMP and cGMP in admixture or both cAMP and cGMP in separate containers.

Journal ArticleDOI
TL;DR: In this paper, the physical conditions necessary to obtain uniform and reproducible chemical reaction rates in an oxygen plasma are investigated by stripping photoresist from silicon wafers, and the results show that at flow rates corresponding to residence times in the range of 1-10 s, diffusion makes the concentration uniform within a few percent except near the walls.
Abstract: The physical conditions necessary to obtain uniform and reproducible chemical reaction rates in an oxygen plasma are investigated by stripping photoresist from silicon wafers. An oxygen plasma was selected due to its simplicity and the availability of a simple technique for measuring the concentration of atomic oxygen which is the reagent of importance. However, many of the considerations will apply to the design of other plasmas for other chemical reactions. Due to the electrical Skin effect at 13.56 MHz, the atomic oxygen is created near the Walls in a cylindrical reactor. However, at flow rates corresponding to residence times in the range of 1-10 s, diffusion makes the concentration uniform within a few percent except near the walls. Under conditions such that there is no by-product inhibition, the chemical reaction rate is determined bythe atomic oxygen concentration and the temperature of the silicon substrate and the reactor walls. The rate is independent of the conbination of pressure and power used to produce the atomic oxygen concentration.


Journal ArticleDOI
TL;DR: The chiral acylating reagent was used in the determination of the enantiomeric composition of 2,5-dimethoxy-4- methylamphetamine excreted in rat urine after intraperitoneal drug administration and may be suitable for the resolution of amino acid enantiomers via the amide derivatives of the methyl esters.

Journal ArticleDOI
TL;DR: A micromethod based on the formation of free fatty acids-copper soaps with a stable copper reagent and sensitive indicator for copper, 2-(2-thiazolylazo)-4-methoxyphenol, is described.