Sulfamic Acid Promoted Expeditious and Column Chromatography Free Synthesis of Functionalized Spiro [indoline-3, 7′-pyrano [3, 2-c: 5, 6-c'] dichromene]-2, 6′, 8′-trione derivatives under Reflux Conditions

2021 ◽  
pp. 132213
Author(s):  
Kajal Mal ◽  
Chhanda Mukhopadhyay
Keyword(s):  
Column Chromatography ◽  
Sulfamic Acid

Heparin Excretion in Intact and Hepatectomized Rats

1981 ◽  
Vol 45 (02) ◽  
pp. 146-149
Author(s):  
Ray Losito ◽  
Harry Gattiker ◽  
Ginette Bilodeau
Keyword(s):  
Column Chromatography ◽  
Normal Values ◽  
Anticoagulant Activity ◽  
Biliary Fistula ◽  
Kinetics Of ◽  
Intact Rats

SummaryMetabolism and kinetics of 3H-heparin were compared in intact and hepatectomized rats. Rats were divided into three groups: 1) intact rats with biliary fistulas and cystostomies 2) intact rats with only cystostomies and 3) hepatectomized rats with cystostomies. Radioactivity in blood, bile and urine besides anticoagulant activity in blood and urine were examined. In addition, column chromatography of urine was used to isolate possible metabolites. Seventy percent and 80% of the radioactive dose was found in the urine of intact rats at 24 hr and 48 hr. Close to 5% of the radioactivity was found in bile or rats with a biliary fistula after 48 hr. The APTT declined to near normal values at 1 hr whether rats had a biliary fistula or not. In contrast, only 25 % of the radioactivity could be excreted into the urine of hepatectomized rats in 24 hr; the APTT did not decline as fast and at 5 hr, it was still 100 seconds. Only one radioactive component could be isolated on chromatography from all urines of these animals and appears to be similar to the original heparin. Thus, the liver has an important role to play in regulating the anticoagulant effects and excretion of heparin.

Identification of acid-insoluble filter-plugging compounds and optimal acid-washing procedures for tubular backpulse pressure filters

TAPPI Journal ◽  
2011 ◽  
Vol 10 (1) ◽  
pp. 17-23
Author(s):  
KEVIN TAYLOR ◽  
RICH ADDERLY ◽  
GAVIN BAXTER
Keyword(s):  
Calcium Sulfate ◽  
Membrane Filter ◽  
Sulfamic Acid ◽  
Xrd Analysis ◽  
Metal Sulfides ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gypsum Formation ◽  
Acid Washing ◽  
Hydrolysis Of

Over time, performance of tubular backpulse pressure filters in kraft mills deteriorates, even with regular acid washing. Unscheduled filter replacement due to filter plugging results in significant costs and may result in mill downtime. We identified acid-insoluble filter-plugging materials by scanning electron microscope/energy-dispersion X-ray spectroscopy (SEM/EDS) and X-ray diffraction (XRD) analysis in both polypropylene and Gore-Tex™ membrane filter socks. The major filter-plugging components were calcium sulfate (gypsum), calcium phosphate (hydroxylapatite), aluminosilicate clays, metal sulfides, and carbon. We carried out detailed sample analysis of both the standard acid-washing procedure and a modified procedure. Filter plugging by gypsum and metal sulfides appeared to occur because of the acid-washing procedure. Gypsum formation on the filter resulted from significant hydrolysis of sulfamic acid solution at temperatures greater than 130°F. Modification of the acid-washing procedure greatly reduced the amount of gypsum and addition of a surfactant to the acid reduced wash time and mobilized some of the carbon from the filter. With surfactant, acid washing was 95% complete after 40 min.

VANILLINSÄURE ALS ENDPRODUKT DES STOFFWECHSELS VON ADRENALIN UND NORADRENALIN. II.

1963 ◽  
Vol 44 (1) ◽  
pp. 101-106 ◽  
Author(s):  
Wilhelm Dirscherl ◽  
Helmut Thomas
Keyword(s):  
Rat Liver ◽  
Paper Chromatography ◽  
Column Chromatography ◽  
Vanillic Acid ◽  
Hippuric Acid ◽  
Single Spot ◽  
Solvent Systems ◽  
Perfusion Experiment ◽  
Kinetics Of

ABSTRACT Perfusion of rat liver with vanillic acid yielded only one metabolite. In paper chromatography with three different solvent systems, the substance showed the same RF-values as vanillyolglycine (3-methoxy-4-hydroxyhippuric acid) and in mixed chromatograms there was only one single spot. After separation by column chromatography, the UV- and IRspectra of the reaction product were identical with those of 3-methoxy4-hydroxy-hippuric acid. During the perfusion experiment, the kinetics of the conjugation were investigated.

DIE ZUSAMMENSETZUNG DER JODHALTIGEN VERBINDUNGEN UND IHRE BEZIEHUNG ZUM JODUMSATZ IN EUTHYREOTEN STRUMEN

1962 ◽  
Vol 41 (4) ◽  
pp. 584-594 ◽  
Author(s):  
Dankwart Reinwein ◽  
Erich Klein
Keyword(s):  
Column Chromatography ◽  
Iodine Content ◽  
High Plasma ◽  
Secretion Rate ◽  
Total Iodine ◽  
Iodine Compound ◽  
Hormonal Secretion ◽  
Carrier Free ◽  
Iodine Metabolism ◽  
Diffuse Goiter

ABSTRACT The iodine metabolism was investigated in 29 patients with euthyroid non-endemic diffuse goiter. 1 to 14 days before thyroidectomy the patients received carrier-free 131I. The chemical iodine fractions (PBI, BEI and iodide) of the thyroid and the labelled iodine compound were analyzed by means of paper- and column chromatography. In one gland the total iodine content varied only by ± 19.6% of the average, the relative shares of PBI, BEI and iodide as well as that of the iodoamino acids being equal. Monoiodotyrosine, diiodotyrosine and thyroxine were found in the thyroid homogenate without hydrolysis. The homogenate after hydrolysis contained more iodotyrosines at the expense of iodothyronines than do normal glands. 17 goiters with normal 131I-uptake showed a high total iodine content (14.2 ± 5.0 mg) whilst 9 goiters with an increased 131I-uptake had low values (3.58 ± 0.6 mg). The opposite was found for the relative shares of BEI with the chromatographically isolated iodothyronines thyroxine, triiodothyronine and an unidentified iodine compound. Goiters with »high plasma PB131I« were characterized by a faster transfer of 131I into the more heavily iodinated compounds than is found in glands with a normal hormonal secretion rate. The highest values for the iodothyronines were found in goiters with increased 131I-uptake together with a high hormonal secretion rate. From this study it appears that the changes in the iodine-poor glands are due to a defective exo- or endogenous iodine supply. The observed alterations in iodine-rich glands are probably induced by a faulty iodine utilization characterized by an incomplete iodotyrosyl-coupling defect.

A technique for uranium and plutonium determination using coulometric potentiostatic facility UPK-19 for analysis of mixed-oxide fuel

2020 ◽  
Vol 86 (12) ◽  
pp. 15-22
Author(s):  
N. A. Bulayev ◽  
E. V. Chukhlantseva ◽  
O. V. Starovoytova ◽  
A. A. Tarasenko
Keyword(s):  
Acid Solution ◽  
Mass Fraction ◽  
Background Electrolyte ◽  
Stable State ◽  
Sulfamic Acid ◽  
Oxide Fuel ◽  
Oxidation Current ◽  
Mox Fuel ◽  
Mass Fractions ◽  
Uranium Plutonium

The content of uranium and plutonium is the main characteristic of mixed uranium-plutonium oxide fuel, which is strictly controlled and has a very narrow range of the permissible values. We focused on developing a technique for measuring mass fractions of uranium and plutonium by controlled potential coulometry using a coulometric unit UPK-19 in set with a R-40Kh potentiostat-galvanostat. Under conditions of sealed enclosures, a special design of the support stand which minimized the effect of fluctuations in ambient conditions on the signal stability was developed. Optimal conditions for coulometric determination of plutonium and uranium mass fractions were specified. The sulfuric acid solution with a molar concentration of 0.5 mol/dm3 was used as a medium. Lead ions were introduced into the background electrolyte to decrease the minimum voltage of hydrogen reduction to –190 mV. The addition of aluminum nitride reduced the effect of fluoride ions participating as a catalyst in dissolving MOX fuel samples, and the interfering effect of nitrite ions was eliminated by introducing a sulfamic acid solution into the cell. The total content of uranium and plutonium was determined by evaluation of the amount of electricity consumed at the stage of uranium and plutonium co-oxidation. Plutonium content was measured at the potentials, at which uranium remains in the stable state, which makes it possible to subtract the contribution of plutonium oxidation current from the total oxidation current. The error characteristics of the developed measurement technique were evaluated using the standard sample method and the real MOX fuel pellets. The error limits match the requirements set out in the specifications for MOX fuel. The technique for measuring mass fractions of uranium and plutonium in uranium-plutonium oxide nuclear fuel was certified. The relative measurement error of the mass fraction of plutonium and uranium was ±0.0070 and ±0.0095, respectively. The relative error of the ratio of the plutonium mass fraction to the sum of mass fractions of uranium and plutonium was ±0.0085.

Protein Solvent Interaction: Transition of Protein-solvent Interaction Concept from Basic Research into Solvent Manipulation of Chromatography

2018 ◽  
Vol 20 (1) ◽  
pp. 34-39 ◽  
Author(s):  
Tsutomu Arakawa ◽  
Yoshiko Kita
Keyword(s):  
Column Chromatography ◽  
Rapid Development ◽  
Academic Research ◽  
Basic Research ◽  
Protein Stabilization ◽  
Special Issue ◽  
Solvent Interaction ◽  
Protein Formulations ◽  
Solvent Additive ◽  
Downstream Processes

Previously, we have reviewed in this journal (Arakawa, T., Kita, Y., Curr. Protein Pept. Sci., 15, 608-620, 2014) the interaction of arginine with proteins and various applications of this solvent additive in the area of protein formulations and downstream processes. In this special issue, we expand the concept of protein-solvent interaction into the analysis of the effects of solvent additives on various column chromatography, including mixed-mode chromatography. Earlier in our research, we have studied the interactions of such a variety of solvent additives as sugars, salts, amino acids, polymers and organic solvents with a variety of proteins, which resulted in mechanistic understanding on their protein stabilization and precipitation effects, the latter known as Hofmeister series. While such a study was then a pure academic research, rapid development of genetic engineering technologies and resultant biotechnologies made it a valuable knowledge in fully utilizing solvent additives in manipulation of protein solution, including column chromatography.

Zinc Sulfamate Catalyzed Efficient Selective Synthesis of Benzimidazole Derivatives under Ambient Conditions

2019 ◽  
Vol 16 (9) ◽  
pp. 740-749
Author(s):  
Sushil R. Mathapati ◽  
Arvind H. Jadhav ◽  
Mantosh B. Swami ◽  
Jairaj K. Dawle
Keyword(s):  
Benzimidazole Derivative ◽  
Sulfamic Acid ◽  
Aromatic Aldehydes ◽  
Catalytic Amount ◽  
Product Yield ◽  
Lewis Acidity ◽  
Benzimidazole Derivatives ◽  
Ambient Conditions ◽  
Reaction Condition ◽  
Green Approach

Zinc sulfamate (Zn(NH2SO3)2 is a derivative of sulfamic acid (H3NSO3) which possesses “Lewis acidity” and finds well suited in a number of catalytic applications. The present paper describes an efficient, eco-friendly, and clean synthesis of 2-substituted benzimidazole derivatives by reacting diverse o-phenylenediamine with various substituted aromatic aldehydes using a catalytic amount of zinc sulfamate in ethanol at ambient temperature. As a result, 10 mol.% of Zinc sulfamate catalyst showed 92% of respective product yield with 100% conversion using short reaction period in ethanol. Meanwhile, effect of reaction parameters, such as amount of catalyst, different solvents, and reaction temperature on reaction product, was also studied. In addition, in the optimized reaction condition various substituted biological important benzimidazoles derivatives were prepared by using optimized reaction condition in good to efficient yield. In addition, possible reaction mechanism in the presence of zinc sulfamate for the preparation of benzimidazole derivative was sketched and discussed. The present green approach showed significances with faster reaction rate with inexpensive catalyst, which showed excellent and clean yield of benzimidazole in mild reaction condition with easy work-up procedure.

A Cytotoxic Natural Product from Patrinia villosa Juss

2019 ◽  
Vol 19 (11) ◽  
pp. 1399-1404 ◽  
Author(s):  
Yangcheng Liu ◽  
Wei Liu ◽  
Changlan Chen ◽  
Zheng Xiang ◽  
Hongwei Liu
Keyword(s):  
Cell Cycle ◽  
Cell Lines ◽  
Silica Gel ◽  
Column Chromatography ◽  
Bioactive Compound ◽  
Antitumor Agent ◽  
2D Nmr ◽  
Preparative Hplc ◽  
Dependent Manner ◽  
2D Nmr Spectra

Background and Purpose:: Patrinia villosa Juss is an important Chinese herbal medicine widely used for thousands of years, but few reports on the ingredients of the herb have been presented. In this study, we aim to isolate the bioactive compound from the plant. Material and Methods:: The air-dried leaves of P. villosa (15kg) were extracted three times with 70% EtOH under reflux. The condensed extract was suspended in H2O and partitioned with light petroleum, dichloromethane and n-BuOH. The dichloromethane portion was then subjected to normal-phase silica gel column chromatography, ODS silica gel column chromatography and semi-preparative HPLC to yield compound 1. Cytotoxicities of 1 were assayed on HepG2, A549 and A2780 cell lines. The mechanism of apoptosis and cell cycle on A549 was confirmed subsequently. Results: A new impecylone (Impecylone A) was isolated from the leaves of Patrinia villosa Juss, and its structures were established using 1D, 2D-NMR spectra and HR-ESI-MS. Impecylone A could selectivity inhibit HepG2 and A549 cell lines. The compound could induce apoptosis of A549 and arrest the cell cycle at G2/M phase in a dose-dependent manner. Conclusion: Impecylone A is a novel compound from Patrinia villosa Juss and could be a potential antitumor agent especially in the cell lines of A549.

Isolation of Sinapic Acid from Habenaria intermedia D. Don: A New Chemical Marker for the Identification of Adulteration and Substitution

2020 ◽  
Vol 6 (4) ◽  
pp. 380-387
Author(s):  
Jaswinder Kaur Virk ◽  
Vikas Gupta ◽  
Mukesh Maithani ◽  
Ravindra K. Rawal ◽  
Sanjiv Kumar ◽  
...  
Keyword(s):  
Column Chromatography ◽  
Sinapic Acid ◽  
Phytochemical Screening ◽  
Chemical Marker ◽  
Reference Compound ◽  
Crystalline Powder ◽  
Chemical Test ◽  
Herbal Plants ◽  
Single Compound ◽  
Layer Chromatography

Background: Vriddhi is one of the Rasayana herbs in Ayurveda broadly used in vitality, strengthening Ayurvedic formulations. To fulfill steeply increased demand and declined supply, tubers have been collected in destructive manner resulting in reduced plant population and pushing the plant in Red list of IUCN endangered species. However, manufacturers are using substitutes and other substandard drugs leading to adulteration which puts the importance of therapeutically rich herbal plants at stake. Lack of chemical markers is the main inability of regulatory authorities for not taking any action against this adulteration. Objective: Isolation of chemical marker of plant that can be used as a reference compound for identification of unauthorized substitution. Methods: Preliminary phytochemical screening of methanolic and toluene extract of H. intermedia D. Don was done using standard methods followed by column chromatography for the isolation of phytoconstituents. A total of 3004 fractions were collected with Thin Layer Chromatography (TLC) profiling and different fractions were pooled. A single compound was isolated and confirmed by chemical test, melting point, spectral analysis and compared with the literature. Results: Phytochemical screening of extracts shows the presence of alkaloids, carbohydrates, steroids, terpenoids, flavonoids, tannins and phenolics. A pure white crystalline powder was isolated by column chromatography which was characterized as 3,5-dimethoxy-4- hydroxycinnamic acid (Sinapic acid) with the help of IR and Mass spectroscopy. Conclusion: This is the first report of Sinapic acid as a novel compound from Vriddhi, Habenaria genus and Orchidaceae family. It can be used as a marker for the identification of unauthorized substitution and adulteration claiming the use of Vriddhi.

Sign in / Sign up

Export Citation Format

Share Document