scholarly journals Identification and Quantitation of Polymyxin B, Framycetin, and Dexamethasone in an Ointment by Using Thin-Layer Chromatography with Densitometry

2005 ◽  
Vol 88 (5) ◽  
pp. 1549-1554 ◽  
Author(s):  
Jan Krzek ◽  
Anna Maślanka ◽  
Pawel Lipner
Keyword(s):  
Thin Layer ◽  
Silica Gel ◽  
Polymyxin B ◽  
Rapid Identification ◽  
Mobile Phases ◽  
Relative Standard ◽  
Dexamethasone Acetate ◽  
Similar Accuracy ◽  
Layer Chromatography

Abstract A new thin-layer chromatographic-densitometric method has been developed for rapid identification and quantitative determination of polymyxin B, framycetin, and dexamethasone in a dental ointment. Silica gel 60 and F254 silica gel 60 plates were used for separating antibiotics and dexamethasone acetate, respectively. When determining framycetin and polymyxin B, chromatograms were developed by using 2 mobile phases, namely methanol and methanol–n-butanol–ammonia (25%)–chloroform (14 + 4 + 9 + 12, v/v/v/v/). The densitometric measurements were made at 550 nm after detection with 0.3% ninhydrin solution. Dexamethasone was determined by using the mobile phase cyclohexane–ethyl acetate (2 + 3, v/v) and ultraviolet densitometric recording at 245 nm. The results obtained for individual constituents with the chromatographic-densitometric method demonstrate similar accuracy, relative standard deviation values from 1.49 to 2.47%, and relative error values from 0.02 to 0.81% and are comparable to those obtained with the reference methods.

scholarly journals Normal and reversed phase thin-layer chromatography of new 16, 17-secoestrone derivatives

2003 ◽  
Vol 68 (1) ◽  
pp. 57-64 ◽  
Author(s):  
Marijana Acanski ◽  
Suzana Jovanovic-Santa ◽  
Lidija Jevric
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Reversed Phase ◽  
Retention Behavior ◽  
Mobile Phases ◽  
Layer Chromatography

The retention behavior and separation ability of a series of new 16,17-secoestrone derivatives has been studied on silica gel, alumina and C-18 silica gel layers with non-aqueous and aqueous-organic mobile phases. The retention behavior and separation ability are discussed in terms of the nature of the solute, eluent and stationary phase.

The Identification of Rubber Compounding Ingredients by Using Thin Layer Chromatography

1983 ◽  
Vol 56 (5) ◽  
pp. 1080-1095 ◽  
Author(s):  
B. J. Gedeon ◽  
T. Chu ◽  
S. Copeland
Keyword(s):  
Molecular Weight ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Easy Method ◽  
Mobile Phases ◽  
Rf Values ◽  
Visualization Systems ◽  
Layer Chromatography

Abstract TLC is a quick, easy method to the identification of rubber compounding ingredients. Both silica gel absorbent and C18 absorbent are suitable for these identifications. With the mobile phases used in this study, a better separation of antioxidants is possible using silica gel absorbent. Work should be continued on finding suitable mobile phases for the C18 absorbent, since the Rf values are more reproducible. For those separations that require a separation of compounds of varying molecular weight, the C18 absorbent is superior to silica gel absorbent. The visualization systems that have been developed for use with silica gel absorbent are suitable for use with C18 absorbent. These systems give the same colors for either absorbent.

scholarly journals Quantitative Determination of Triterpenes from Amphiptherygium adstringens by Liquid Chromatography and Thin-Layer Chromatography and Morphological Analysis of Cuachalalate Preparations

2006 ◽  
Vol 89 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Andrés Navarrete ◽  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Xiuhong Ji ◽  
Paul Hersh ◽  
...  
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Gastric Ulcers ◽  
Array Detector ◽  
Plant Materials ◽  
Relative Standard ◽  
Layer Chromatography

Abstract Amphiptherygium adstringens (Anacardiaceae/Julianaceae), local name cuachalalate, is used in folk medicine for the treatment of cholelithiasis, fevers, fresh wounds, hypercholesterolemia, gastritis, gastric ulcers, and cancer of the gastrointestinal tract. The development of column high-performance liquid chromatographyphotodiode array detector (LC-PDA) and high-performance thin-layer chromatography (HPTLC)densitometry methods for the determination of masticadienonic acid and 3-hydroxymasticadienonic acid in cuachalalate preparations is described in this paper. Good separation of the compounds could be achieved by both methods. Either might be preparable depending on the requirements. The LC separation was performed on a Phenomenex Synergi MAX-RP 80A reversed-phase column operated at 40C with detection at 215 nm. The plant materials were extracted with methanol by sonication. The triterpenes present in the plant material and commercial extracts were separated with an acetonitrilewater reagent alcohol isocratic system. The limit of detection was 0.10.2 g/mL. The relative standard deviation values for the determination of triterpenes in plant extracts were less than 1.00%. This is the first report of an analytical method developed for the quantitative analysis of triterpenes from Amphiptherygium adstringens by LC-PDA and HPTLC. The stem bark showed higher amounts of triterpenes, and low amounts in root and stem root. The microscopic description of the crude drug of cuachalalate was also provided.

Toxigenic isolates of Fusarium sporotrichioides obtained from hay in Saskatchewan

1982 ◽  
Vol 28 (2) ◽  
pp. 259-261 ◽  
Author(s):  
G. R. F. Davis ◽  
N. D. Westcott ◽  
J. D. Smith ◽  
G. A. Neish ◽  
H. B. Schiefer
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Western Canada ◽  
Fusarium Sporotrichioides ◽  
Insect Larvae ◽  
Main Band ◽  
Rats And Mice ◽  
Layer Chromatography

An isolate of Fusarium sporotrichioides Sherbakoff obtained from hay from Kindersley, Saskatchewan, and producing metabolites toxic to insect larvae, rats, and mice was cultured on sterile rye grain and extracted with ethyl acetate. The most toxic fraction derived from column chromatography on silica gel was purified by thin-layer chromatography on silica gel and elution of the main band. This compound was identified as T-2 toxin by comparison with the pure chemical by thin-layer chromatography and, after crystallization, by determination of melting point, infrared spectrum, and nuclear magnetic resonance spectrum. This work demonstrates that strains of F. sporotrichioides capable of producing T-2 toxin may be present on hay in western Canada.

Determination of Aflatoxins in Animal Tissues

1981 ◽  
Vol 64 (4) ◽  
pp. 964-968
Author(s):  
Robert D Stubblefield ◽  
Odette L Shotwell
Keyword(s):  
Citric Acid ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Determination Limit ◽  
Animal Tissues ◽  
Freeze Dried ◽  
Human Livers ◽  
Layer Chromatography

Abstract A method for the determination of aflatoxins in animal tissues has been developed, and applied successfully to beef, swine, chicken, and human livers, and to beef kidney, heart, spleen, muscle, and blood. Blended tissue is denatured with citric acid and extracted with dichloromethane on a wrist-action shaker. After filtration, the extract is partially purified on a silica gel column, and aflatoxins B1 and M1 are determined by 2-dimensional thin layer chromatography and densitometry. Recoveries of Bi and Mi added to meat tissues and blood were approximately 90 and 80%, respectively. The method gave results for a contaminated freeze-dried liver comparable to analyses by 3 other published meat tissue methods. The method is rapid and has a determination limit ≤0.1 ng/g. In addition, the method uses less toxic and smaller quantities of solvents and chemicals.

scholarly journals Determination of mono- and diacylglycerols from E 471 food emulsifiers in aerosol whipping cream by high-performance thin-layer chromatography–fluorescence detection

2020 ◽  
Vol 412 (27) ◽  
pp. 7441-7451
Author(s):  
Claudia Oellig ◽  
Max Blankart ◽  
Jörg Hinrichs ◽  
Wolfgang Schwack ◽  
Michael Granvogl
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Food Additives ◽  
German Market ◽  
Relative Standard ◽  
Model Aerosol ◽  
Layer Chromatography

Abstract Mono- and diacylglycerol (MAG and DAG) emulsifiers (E 471) are widely applied to regulate techno-functional properties in different food categories, for example, in dairy products. A method for the determination of MAG and DAG in aerosol whipping cream by high-performance thin-layer chromatography with fluorescence detection (HPTLC–FLD) after derivatization with primuline was developed. For sample preparation, aerosol whipping cream was mixed with ethanol, followed by the addition of water and liquid-liquid extraction with tert-butyl methyl ether. The sample extracts were analyzed by HPTLC–FLD on silica gel LiChrospher plates with n-pentane/n-hexane/diethyl ether (22.5:22.5:55, v/v/v) as mobile phase, when interfering matrix like cholesterol and triacylglycerols were successfully separated from the E 471 food additives. For quantitation, an emulsifier with known composition was used as calibration standard and the fluorescent MAG and DAG were scanned at 366/> 400 nm. Limits of detection and quantitation of 4 and 11 mg/100 g aerosol whipping cream were obtained for both monostearin and 1,2-distearin, respectively, and allowed the reliable quantitation of MAG and DAG from E 471 far below commonly applied emulsifier amounts. Recoveries from model aerosol whipping cream with 400 mg E 471/100 g were determined in a calibration range of 200–600 mg E 471/100 g sample and ranged between 86 and 105% with relative standard deviations below 7%. In aerosol whipping creams from the German market, E 471 amounts ranged between 384 and 610 mg/100 g.

scholarly journals Identification and Determination of Oxytetracycline, Tiamulin, Lincomycin, and Spectinomycin in Veterinary Preparations by Thin-Layer Chromatography/Densitometry

2000 ◽  
Vol 83 (6) ◽  
pp. 1502-1506 ◽  
Author(s):  
Jan Krzek ◽  
Anna Kwiecień ◽  
Małgorzata Starek ◽  
Anna Kierszniewska ◽  
Włodzimierz Rzeszutko
Keyword(s):  
Quantitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Citric Acid Solution ◽  
Active Constituents ◽  
Mobile Phases ◽  
Rf Values ◽  
Layer Chromatography ◽  
Small Confidence Interval

Abstract A thin-layer chromatographic/densitometric method was developed for the identification and quantitation of oxytetracycline, tiamulin, lincomycin, and spectinomycin in veterinary preparations. Silica gel-coated thin layer chromatography plates and 2 mobile phases were used to separate these constituents. The appropriate compositions of the suitable mobile phases were established: 10% citric acid solution–n-hexane–ethanol (80 + 1 + 1, v/v) and n–butanol–ethanol–chloroform– 25% ammonia (4 + 5 + 2 + 5, v/v). Along with Rf values and spot colors, direct UV and visual densitometric measurements were used for identification. Similar measuring ranges were used for quantitative analysis to obtain repeatable and reliable results for the preparations examined. The results of the quantitative analysis are characterized by a small confidence interval and are close to the declared contents of active constituents: oxytetracycline 30.01 ± 0.38 g at λ = 350 nm and 30.24 ± 0.86 g at λ = 430 nm; tiamulin, 10.19 ± 0.86 g at λ = 450 nm; lincomycin, 2.27 ± 0.08 g at λ = 278 nm; and spectinomycin, 2.18 ± 0.07 g at λ = 421 nm. The recoveries for all antibiotics ranged from 100.01 to 102.54%.

Improved Method for the Thin Layer Chromatographic Determination of Patulin in Apple Juice

1973 ◽  
Vol 56 (4) ◽  
pp. 813-816 ◽  
Author(s):  
Peter M Scott ◽  
Barry P C Kennedy
Keyword(s):  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Apple Juice ◽  
Chromatographic Determination ◽  
Improved Method ◽  
Layer Chromatography ◽  
Hydrochloride Solution

Abstract Apple juice from a freshly opened container is extracted 3 times with ethyl acetate. The extract is dried, concentrated, diluted with benzene, and added to a silica gel column. Patulin is eluted by benzene-ethyl acetate (75+25) and detected by thin layer chromatography, using a 3-methyl-2-benzothiazolinone hydrazone hydrochloride solution as the spray reagent. Satisfactory recoveries were obtained for patulin added to apple juice at levels of 25–400 μg/L.

scholarly journals Development of Chromatographic Methods for Determination of Agrimoniin and Related Polyphenols in Pharmaceutical Products

2009 ◽  
Vol 92 (2) ◽  
pp. 410-418 ◽  
Author(s):  
Izabela Fecka
Keyword(s):  
Silica Gel ◽  
Extraction Procedure ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Mobile Phases ◽  
Sample Extraction ◽  
Unmodified Silica ◽  
Short Time ◽  
Layer Chromatography

Abstract Thin-layer chromatography (TLC) and liquid chromatography (LC) methods were developed for the qualitative and quantitative determination of agrimoniin, pedunculagin, ellagic acid, gallic acid, and catechin in selected herbal medicinal products from Rosaceae: Anserinae herba, Tormentillae rhizoma, Alchemillae herba, Agrimoniae herba, and Fragariae folium. Unmodified silica gel (TLC Si60, HPTLC LiChrospher Si60) and silica gel chemically modified with octadecyl or aminopropyl groups (HPTLC RP18W and HPTLC NH2) were used for TLC. The best resolution and selectivity were achieved with the following mobile phases: diisopropyl etheracetoneformic acidwater (40 30 20 10, v/v/v/v), tetrahydrofuranacetonitrilewater (30 10 60, v/v/v), and acetoneformic acid (60 40, v/v). Concentrations of the studied herbal drugs were determined by using a Chromolith Performance RP-18e column with acetonitrilewaterformic acid as the mobile phase. Determinations of linearity, range, detection and quantitation limits, accuracy, precision, and robustness showed that the HPLC method was sufficiently precise for estimation of the tannins and related polyphenols mentioned above. Investigations of suitable solvent selection, sample extraction procedure, and short-time stability of analytes at storage temperatures of 4 and 20C were also performed. The percentage of agrimoniin in pharmaceutical products was between 0.57 and 3.23.

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.

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