scholarly journals THE SULFONATION STUDY OF REACTION MECHANISM ON PAPAVERINE ALKALOID BY GC-MS AND FT-IR

2010 ◽  
Vol 7 (1) ◽  
pp. 67-71
Author(s):  
I Made Sudarma
Keyword(s):  
Reaction Mechanism ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Sulfonyl Chloride ◽  
The Other ◽  
Sulfonyl Group ◽  
Molecular Ion ◽  
Ft Ir ◽  
Theoretical Mechanism ◽  
Layer Chromatography

The aim of this research was to prove theoretical mechanism reaction on the sulfonation of papaverine alkaloid and the result could be used as a reference on the transformation of these alkaloid to the other derivatives. Theoriticaly sulfonation of papaverine (1) by HO-SO2Cl could produced papaverine sulfonyl chloride (1a). The formation of this product was analyzed by analytical thin layer chromatography GC-MS, and FT-IR. These analysis showed the formation of product (1a) more favorable than the other. Tlc showed product (1a) less polar than papaverine, and supported by GC-MS and infrared which showed molecular ion at m/z 412 due to the presence of -SO2Cl and vibration at 1153,4 dan 1265,2 Cm-1 due to absorption of sulfonyl group.   Keywords: reaction mechanism, sulfonation, papaverine alkaloid.

Sugar-meal sources used by female black flies (Diptera: Simuliidae): a four-habitat study

1997 ◽  
Vol 75 (7) ◽  
pp. 1066-1072 ◽  
Author(s):  
Steven G. Burgin ◽  
Fiona F. Hunter
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
The Other ◽  
Black Flies ◽  
Layer Chromatography ◽  
Provincial Park

Adult black flies were sampled by sweep-netting vegetation in four habitats within Algonquin Provincial Park, Ontario: Davies Bog, the airfield, deciduous habitat, and coniferous habitat. Sugars in the crops and midguts of female flies (n = 773) were tested by thin-layer chromatography to determine whether the flies had fed on nectar or homopteran honeydew. Melezitose and stachyose were used as honeydew-indicator sugars. For Simulium venustum, it was found that significantly fewer black flies (19%) from the airfield contained honeydew sugars than black flies from the other three sites (34% from Davies Bog; 36% from deciduous habitat; 25% from coniferous habitat). We argue that black flies will feed on nectar or honeydew according to availability.

scholarly journals 5α-Androstane-3α,17β-Diol Is Formed in Tammar Wallaby Pouch Young Testes by a Pathway Involving 5α-Pregnane-3α,17α-Diol-20-One as a Key Intermediate

Endocrinology ◽  
2003 ◽  
Vol 144 (2) ◽  
pp. 575-580 ◽  
Author(s):  
Jean D. Wilson ◽  
Richard J. Auchus ◽  
Michael W. Leihy ◽  
Oleg L. Guryev ◽  
Ronald W. Estabrook ◽  
...  
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Reductase Inhibitor ◽  
Tammar Wallaby ◽  
The Other ◽  
Synthetic Pathway ◽  
D 20 ◽  
17 Hydroxyprogesterone ◽  
Layer Chromatography

The synthetic pathway by which 5α-androstane-3α,17β-diol (5α-adiol) is formed in the testes of tammar wallaby pouch young was investigated by incubating testes from d 20–40 males with various radioactive precursors and analyzing the metabolites by thin-layer chromatography and HPLC. [3H]Progesterone was converted to 17-hydroxyprogesterone, which was converted to 5α-adiol by two pathways: One involves the formation of testosterone and dihydrotestosterone as intermediates, and the other involves formation of 5α-pregnane-3α,17α-diol-20-one (5α-pdiol) and androsterone as intermediates. Formation of 5α-adiol from both [3H]testosterone and [3H]progesterone was blocked by the 5α-reductase inhibitor 4MA. The addition of nonradioactive 5α-pdiol blocked the conversion of [3H]progesterone to 5α-adiol, and [3H]5α-pdiol was efficiently converted to androsterone and 5α-adiol. We conclude that expression of steroid 5α-reductase in the developing wallaby testes allows formation of 5α-reduced androgens by a pathway that does not involve testosterone as an intermediate.

scholarly journals Separation of Berberine Hydrochloride and Tetrahydropalmatine and Their Quantitative Analysis with Thin Layer Chromatography Involved with Ionic Liquids

2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Jing Lu ◽  
Hong-yan Ma ◽  
Wei Zhang ◽  
Zhi-guo Ma ◽  
Shun Yao
Keyword(s):  
Ionic Liquids ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Simple Procedure ◽  
Berberine Hydrochloride ◽  
Chinese Patent ◽  
Ft Ir ◽  
First Time ◽  
Layer Chromatography

[BMIM]OH was used in mobile and stationary phase of thin layer chromatography (TLC) to analyze berberine hydrochloride and tetrahydropalmatine for the first time. Supported imidazole ionic liquid with hydroxide ion on silica gel (SiO2·Im+·OH−) was synthesized through simple procedure and characterized by Fourier transform infrared spectroscopy (FT-IR), elemental analysis, and scanning electron microscope (SEM). Moreover, on the plates prepared by SiO2·Im+·OH−, the contents of the above alkaloids in the Chinese patent medicine (CPM) of “Stomacheasy” capsule were successfully determined by TLC scanner. The key conditions and chromatographic behaviors were also investigated in detail. According to similar ways, ionic liquids (ILs) also can be used in other planar chromatographies in two modes. This study is expected to be helpful in expanding the application of IL and its bonded silica gel in TLC separation field.

Platelet Factor 3 Activity in Washed Platelets

1973 ◽  
Vol 30 (03) ◽  
pp. 557-566 ◽  
Author(s):  
S Renaud ◽  
P Gautheron ◽  
H Rosenstein
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Platelet Rich Plasma ◽  
The Other ◽  
Slow Speed ◽  
Platelet Factor ◽  
Platelet Poor Plasma ◽  
Platelet Counts ◽  
Edta Solution ◽  
Layer Chromatography

SummaryPlatelets collected with an EDTA solution and simply washed in an incomplete Tyrode’s presented clotting times in the recalcification (man and rat) and the Stypven (rat) tests that were practically identical to those of the PRP when slow speed centrifugation was used (800 G in man, 1000 G in rat). This was demonstrated, in 6 pools of 5 rats each and in 6 men, by comparing the clotting activity of the citrated platelet-rich plasma to that of the platelets washed and resuspended in the citrated platelet-poor plasma, for platelet counts ranging from 1 × 105 to 10 × 105/mm3. In contrast, centrifugation of platelets at 3000 G markedly affected these clotting activities, as was shown in an additional study comprising 6 pools of 3 rats.Finally, the clotting activity of platelets totally disrupted by sonication appears to be identical quantitatively in both man and rats to that of the total phospholipids extracted from these platelets and separated from the other lipids by thin-layer chromatography and resuspended in plasma by sonication.

Determination of Matacil and Zectran by Fluorigenic Labeling, Thin Layer Chromatography, and In Situ Fluorimetry

1972 ◽  
Vol 55 (6) ◽  
pp. 1259-1264
Author(s):  
R W Frei ◽  
J F Lawrence
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Sulfonyl Chloride ◽  
Relative Standard ◽  
Dansyl Derivatives ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Fluorescent Derivatives

Abstract The fluorigenic labeling of Matacil (4-dimethylamino- m-tolyl N-methylcarbamate) and Zectran (4-dimethylamino-3,5-xylyl Wmethylcarbamate) with dansyl chloride (1-dimethylamino- naphthalene-5-sulfonyl chloride) results in 3 fluorescent derivatives, and labeling with NBD-Cl (4-chloro-7-nitrobenzo- 2,1,3-oxadiazole) produces 2 fluorescent derivatives for each carbamate, all of which can be separated by thin layer chromatography (TLC). These derivatives are identified by nuclear magnetic resonance, infrared, and fluorescence spectroscopy, aided by TLC data. The carbamates are hydrolyzed in dilute base and the resulting amine or phenol hydrolysis products react with the labeling reagents. The derivatives are analyzed by TLC and in situ fluorimetry with a spectrophotometer in the fluorescence mode and a spectrophotofluorometer with the thin layer scanning accessory. Reactions, fluorescence phenomena, and chromatographic properties of the derivatives are investigated for evaluation of the method as a quantitative technique. A reproducibility of 3–5% relative standard deviation can be expected in the concentration range from 15 to 300 ng/spot for derivatives of the 2 labeling procedures. The dansyl derivatives are instrumentally detectable as low as 1 ng/spot while the NBD derivatives may be detected at concentrations of less than 0.5 mg/spot.

Rapid assay of poly(ADP-ribose) glycohydrolase

1987 ◽  
Vol 65 (7) ◽  
pp. 668-673 ◽  
Author(s):  
Luc Ménard ◽  
Guy G. Poirier
Keyword(s):  
Thin Layer ◽  
Enzymatic Activity ◽  
Affinity Chromatography ◽  
Thin Layer Chromatography ◽  
Rapid Method ◽  
The Other ◽  
High Yield ◽  
Rapid Assay ◽  
Layer Chromatography

We have developed a rapid, highly reproducible assay to determine poly(ADP-ribose) glycohydrolase activity which measures directly the appearance of the reaction product. We also analysed the majority of different techniques which are used to determine poly(ADP-ribose) glycohydrolase activity and found that the apparent activity can vary extensively depending on the method used. Thin-layer chromatography using PEI-F–cellulose was the only method which evaluated directly the specific release of ADP-ribose; by comparison with this method, the other procedures gave an over- or under-estimation of 2- to 10-fold of the enzymatic activity. A rapid method of affinity chromatography has also been developed to synthesize and purify in high yield poly(ADP-ribose) (35% conversion of 1 mM NAD to poly (ADP-ribose)).

Production of indole-3-propanoic acid and 3-(p-hydroxyphenyl)propanoic acid by Clostridium sporogenes: a convenient thin-layer chromatography detection system

1980 ◽  
Vol 26 (4) ◽  
pp. 448-453 ◽  
Author(s):  
Joanne J. Jellet ◽  
Thomas P. Forrest ◽  
Ian. A. Macdonald ◽  
Thomas J. Marrie ◽  
Lillian V. Holdeman
Keyword(s):  
Amino Acids ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Detection System ◽  
Spot Test ◽  
The Other ◽  
Propanoic Acid ◽  
Clostridium Sporogenes ◽  
Clostridial Species ◽  
Layer Chromatography

Indole-3-propanoic acid (IPA), 3-(p-hydroxyphenyl)propanoic acid (HPPA), and 3-phenylpropanoic acid (PPA) were present in the spent bacterial media of Clostridium sporogenes (20/20 strains) and C. cylindrosporum (1/1 strains), but absent in 32 other clostridial species (74 strains) tested. Both IPA and HPPA (but not PPA) could be readily detected by thin-layer chromatography and p-hydroxybenzaldehyde spray reagent. IPA forms a scarlet complex with p-hydroxybenzaldehyde which shifts to purple and remains stable for up to 6 weeks. IPA can be detected in acidified extracts of C. sporogenes by a simple spot test. The structures of IPA and HPPA were confirmed by nuclear magnetic resonance (nmr) and mass spectroscopy and their formation was detected by the absorbance at 280 nm. Addition of one of the precursor amino acids (L-tryptophan, L-tyrosine, or L-phenylalanine) to the medium greatly enhanced formation of the corresponding deaminated acid and depressed the formation of the other two acids. The products IPA, HPPA, and PPA, at 10−3M, and spent bacterial media were negative in the direct Ames's assay for mutagenicity and noncytotoxic towards MRC-S cells.

DIE FLUOROMETRISCHE BESTIMMUNG VON TESTOSTERON, EPITESTOSTERON UND ANDROST-4-EN-3,17-DION NACH DÜNNSCHICHTCHROMATOGRAPHISCHER ISOLIERUNG AUS DEM HARN

1968 ◽  
Vol 58 (3) ◽  
pp. 353-363 ◽  
Author(s):  
W. Hubl ◽  
K. Schollberg
Keyword(s):  
Enzymatic Hydrolysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Complete Separation ◽  
The Other ◽  
Simple Method ◽  
Layer Chromatography

ABSTRACT The authors describe a simple method for determining testosterone, epitestosterone and androstenedione. The method employs enzymatic hydrolysis for glucuronide conjugates, Girard-partition, thin-layer chromatography using alumina and polyamide and fluorometric quantitation of the eluted steroids. By means of TLC on polyamide it is possible to separate (testosterone + epitestosterone) from the other C19-steroids. The complete separation of testosterone from epitestosterone is obtained by TLC on alumina as well as on silicagel G.

Metabolism of Pyrazon in Sugar Beets and Soil

Weed Science ◽  
1969 ◽  
Vol 17 (3) ◽  
pp. 327-331 ◽  
Author(s):  
G. R. Stephenson ◽  
S. K. Ries
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Beta Vulgaris ◽  
Phenyl Ring ◽  
The Other ◽  
Labeled Compounds ◽  
Sugar Beets ◽  
Layer Chromatography

Sugar beets (Beta vulgarisL., var. MSU 126 × 5460) were treated with 5-amino-4-chloro-2-phenyl-3(2H)-pyridazinone (pyrazon) applied to the soil. The pyrazon was labeled with either3H in the phenyl ring, or with14C at the 4 and 5 positions of the pyridazinone ring. The disappearance of pyrazon and the appearance of metabolites in the soil and shoots were examined 1, 2, 4, 6, 8, 12, and 16 weeks after treatment. The total recoverable radioactivity decreased with time, but there was a greater loss of3H-labeled compounds than14C-labeled compounds from the soil. Thin-layer chromatography of the soil and shoot extracts revealed the presence of one metabolite in the soil and three metabolites in the plant. By co-chromatography with known pyrazon derivatives and by comparison of the labeling (14C,3H, or both), the metabolites in the shoot were identified as N-(2-chloro-4-phenyl-3(2H)-pyridazinone)-glucosamine (hereinafter referred to as N-glucosyl pyrazon), 5-amino-4-chloro-3(2H)-pyridazinone (hereinafter referred to as ACP), and ACP-complex. The other moiety in the ACP-complex was not identified. The metabolite in the soil was identified as ACP, and was detectable 2 weeks prior to its appearance in the shoot, suggesting that it was absorbed from the soil.

3-Hydroxy-3-methylglutaryl-CoA lyase deficiency as detected by radiochemical assay in cell extracts by thin-layer chromatography, and identification of three new cases

1990 ◽  
Vol 36 (2) ◽  
pp. 297-303 ◽  
Author(s):  
K M Gibson ◽  
C F Lee ◽  
V Kamali ◽  
K Johnston ◽  
A L Beaudet ◽  
...  
Keyword(s):  
Thin Layer ◽  
Urinary Excretion ◽  
Thin Layer Chromatography ◽  
Coenzyme A ◽  
Clinical Laboratory ◽  
Ketone Bodies ◽  
The Other ◽  
Cultured Fibroblasts ◽  
Cell Extracts ◽  
Layer Chromatography

Abstract In this rapid radiochemical assay for 3-hydroxy-3-methylglutaryl-coenzyme A lyase (I) activity in cell extracts, DL-3[glutaryl-3-14C]hydroxy-3-methylglutaryl-coenzyme A is used as substrate and the radiochemical product, [3-14C]acetoacetic acid, is converted to the more stable [3-14C]-3-hydroxybutyric acid in the presence of added NADH and 3-hydroxybutyrate dehydrogenase. Substrate and product are separated and quantified by thin-layer chromatography on cellulose (solvent system: butanol/water/formic acid, 77:13:10 by vol). All reagents for the assay are commercially available. No detailed column chromatography or spectrophotometry is required. Thus the assay is suited for any clinical laboratory. Using this procedure, we studied cultured fibroblasts or lymphocytes isolated from whole blood from five patients in whom the urinary organic acid profile was suggestive of deficiency of I. Three patients had less than or equal to 18% of control I activity in fibroblast or lymphocyte extracts. The other two had activity within the normal range. In one of the latter cases, urinary excretion of three of the characteristic acids disappeared with age, and 3-hydroxyisovaleric acid excretion was within normal limits. The other case presented with urinary excretion of moderate amounts of all four metabolites and the characteristic absence of urinary ketone bodies. Evidently, confirmatory enzyme studies should be undertaken, even when the profile of urinary organic acids appears definitive for this deficiency.

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