CHROMATOGRAPHIC IDENTIFICATION OF ESTRIOL AND 16,17-EPIESTRIOL AS CONSTITUENTS OF THE URINE OF THE LAYING HEN

1967 ◽  
Vol 45 (4) ◽  
pp. 531-539 ◽  
Author(s):  
R. S. Mathur ◽  
R. H. Common
Keyword(s):  
Reference Material ◽  
Thin Layer ◽  
Solvent System ◽  
Alumina Column ◽  
Hydrophilic Fraction ◽  
Alumina Column Chromatography ◽  
Phenolic Extract ◽  
Solvent Systems ◽  
Layer Chromatography ◽  
Derivatives Of

Presumptive estriol and 16,17-epiestriol fractions were separated from laying hens' urine by subjecting the hydrophilic fraction of the urinary phenolic extract to successive thin-layer chromatography (t.l.c), alumina-column chromatography, further t.l.c, and finally, microsublimation. The presence of estriol in the presumptive estriol fraction was confirmed by comparison of the thin-layer chromatographic behaviors of the phenol and four derivatives thereof with the behaviors of reference estriol and four corresponding derivatives of this reference material each in three different solvent systems. The presence of 16,17-epiestriol in the presumptive 16,17-epiestriol fraction was confirmed by similar comparisons of the presumptive 16,17-epiestriol fraction and five derivatives thereof with reference 16,17-epiestriol and five corresponding derivatives each in three solvent systems; and chromatographic correspondences for two further derivatives were observed in one solvent system each.It is concluded that estriol and 16,17-epiestriol are normal constituents of hens' urine.

OPTIMIZATION OF THIN LAYER CHROMATOGRAPHY METHODS FOR SEPARATION AND IDENTIFICATION OF ANTIDEPRESSANTS IN THEIR MIXTURE

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Solvent System ◽  
Ammonia Solution ◽  
Relative Standard ◽  
Rf Values ◽  
Solvent Systems ◽  
Paroxetine Hydrochloride ◽  
Fluvoxamine Maleate ◽  
Layer Chromatography

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly

scholarly journals Thin Layer Chromatographic Analysis of Food Colorants from Three Morphotypes of Annatto (Bixa orellana L.)

2013 ◽  
Vol 2 (1) ◽  
pp. 7-12
Author(s):  
Hari Pada Seal ◽  
Mohammad Amdad Ali ◽  
Md Usuf Ali ◽  
Mosammat Hasina Akhter ◽  
Fowzia Sultana
Keyword(s):  
Thin Layer ◽  
Chromatographic Analysis ◽  
Mixed Solvent ◽  
Solvent System ◽  
Bixa Orellana ◽  
Solvent Extraction Method ◽  
Solvent Systems ◽  
Carrier Solvent ◽  
Thin Layer Chromatographic Analysis ◽  
Layer Chromatography

This article describes a simple solvent extraction method for the extraction of colorants from the three morphotypes such as, (Morphotype-1 (M1), Morphotype-2 (M2), and Morphotype- 3 (M3) of Annatto (Bixa orellana L.) seeds, and their separation, vivid, and qualitative demonstration by thin-layer chromatography. Several solvent systems (hexane, chloroform, acetone, ethanol, and a mixed-solvent having composition of CHCl3/C2H5OH/CH3COOH (80:2:1)) were applied for extraction of colored components. It was observed that a large portion of colorants was extracted by chloroform. Its effluent was deep brick red in color and transparent. Furthermore, various carrier solvent systems (Benzene-Ethyl acetate) were used to separate the components from the extracts. Carrier solvent system with the ratio of 7:3 was found as superior solvent for chloroform extracts. Three colored-spots were observed for all morphotypes. Among them, the first one was yellow colored having very low polarity and the second and third spots were both redbrick colored having medium and higher polarity respectively. In addition, for M1 no colorless-spot was observed in low and medium polar systems, revealing that the amount of wax and gum were minimum in the extract and superior morphotype among the three. DOI: http://dx.doi.org/10.3329/ijarit.v2i1.13987 Int. J. Agril. Res. Innov. & Tech. 2 (1): 7-12, June, 2012

Deoxynivalenol in Winter Wheat: Thin Layer Chromatographic Method and Survey

1984 ◽  
Vol 67 (1) ◽  
pp. 43-45 ◽  
Author(s):  
Robert M Eppley ◽  
Mary W Trucksess Stanley Nesheim ◽  
Charles W Thorpe ◽  
Garnett E Wood ◽  
Albert E Pohland
Keyword(s):  
Winter Wheat ◽  
Thin Layer ◽  
Chromatographic Method ◽  
Wheat Crop ◽  
Alumina Column ◽  
Sample Extraction ◽  
Alumina Column Chromatography ◽  
Winter Wheat Crop ◽  
Layer Chromatography

Abstract A rapid method for the determination of deoxynivalenol (DON) in wheat was used to analyze 57 wheat samples collected from 4 midwestern states where the winter wheat crop was contaminated with Fusaria. The method involves sample extraction with acetonitrilewater (84 + 16), cleanup by charcoal-alumina column chromatography, and determination by thin layer chromatography (TLC), using an AlClj solution spray and heat to form a fluorescent derivative. Recoveries of DON added to wheat at levels as low as 0.2 μg/g averaged >80%. DON was detected at an average level of 3.6 μg/g; the levels ranged from 0.2 to 9.0 μg/g in 54 of 57 of the wheat samples. The quantity of DON was, in general, proportional to the percentage of total damaged kernels (grade). The chemical identity of DON was confirmed by mass spectrometry after isolation with preparative TLC.

Simplified Qualitative Analysis of Glycerides Derived from Coconut Oil Using Thin Layer Chromatography

2012 ◽  
Vol 506 ◽  
pp. 182-185 ◽  
Author(s):  
Sirikarn Pengon ◽  
Chutima Limmatvapirat ◽  
Sontaya Limmatvapirat
Keyword(s):  
Acetic Acid ◽  
Qualitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Cocos Nucifera ◽  
Coconut Oil ◽  
Solvent System ◽  
Tlc Plates ◽  
Solvent Systems ◽  
Layer Chromatography

Coconut (Cocos nucifera L.) oil is composed predominately of medium-chain triglycerides which have been reported to be beneficial to human health. It also contains free fatty acids (FFAs) which can combine with glycerol to form monoglycerides, diglycerides, and triglycerides. The analysis of FFAs and their glycerides has been proposed to assess the quality of coconut oil used as raw materials in various industrial fields. The aim of this study was to develop the qualitative method for investigation of FFA and their glycerides in coconut oil using thin layer chromatography (TLC). Coconut oil and standards of FFA and their glycerides were chromatographed separately on Silica gel 60 F254 TLC plates using hexane: ether: acetic acid (60:40:1) and hexane: ethyl acetate: acetic acid (60:40:0.5) as solvent systems A and B, respectively. The spots on developing TLC plates were detected and compared using 254-nm UV light and iodine vapor. The results showed that the resolution of solvent system A was better than that of solvent system B. However, both solvent systems were used to confirm the results. The retention factor (Rf) values of the components were in good agreement with their polarity. This method should provide a guideline for qualitative analysis of coconut oil.

Aflatoxins: Improved Resolution by Thin Layer Chromatography

1969 ◽  
Vol 52 (4) ◽  
pp. 669-672 ◽  
Author(s):  
R D Stubblefield ◽  
G M Shannon ◽  
O L Shotwell
Keyword(s):  
Quantitative Analysis ◽  
Relative Humidity ◽  
Qualitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Water Concentration ◽  
Solvent System ◽  
Solvent Systems ◽  
Layer Chromatography ◽  
System Water

Abstract Water was added to solvent systems for TLC of aflatoxins to achieve more reproducible results in laboratories where temperature and relative humidity vary. Resolution of the toxins also improved. Increments of water were added to solvent systems composed of acetone-chloroform (10 + 90, 12 + 88, and 15 + 85, v/v). As the water concentration was increased, separation of aflatoxins B2 and G1 improved. These two toxins are usually the most difficult to resolve in these solvent systems. Separations were the best with wateracetone-chloroform (1.5 + 12 + 88, v/v/v). Water added to methanol-chloroform (3 + 97, v/v) improved resolution of this solvent system but not enough for quantitative analysis, or at times, qualitative analysis. The solvent system water-methanol-ether (1 + 3 + 96, v/v/v) separated aflatoxins as well as water-acetone-chloroform (1.5 + 12 + 88, v/v/v).

DEVELOPMENT OF HPTLC METHOD FOR THE ESTIMATION OF ONDANSETRON AND RANITIDINE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 42-48
Author(s):  
P. J. Patel ◽  
◽  
D. A Shah ◽  
F. A. Mehta ◽  
U. K. Chhalotiya
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
High Performance ◽  
Dosage Form ◽  
Solvent System ◽  
Rf Values ◽  
Layer Chromatography ◽  
Hptlc Method

A simple, sensitive and precise high performance thin layer chromatographic (HPTLC)method has been developed for the estimation of ondansetron (OND) and ranitidine (RAN) in combination. The method was employed on thin layer chromatography (TLC) and aluminium plates were precoated with silica gel 60 F254 as the stationary phase, while the solvent system was methanol. The Rf values were observed to be 0.5 ± 0.02, and 0.3 ± 0.02 for OND and RAN, respectively. The separated spots were densitometrically analyzed in absorbance mode at 299 nm. This method was linear in the range of 25-300 ng/band for OND and 50-600 ng/band for RAN. The limits of detection for OND and RAN were found to be 3.47 and 1.83 ng/band, respectively. The limits of quantification for OND and RAN were found to be 10.53 and 5.55 ng/band, respectively. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of OND and RAN in combined dosage form.

EXPERIMENTAL PRODUCTION OF AFLATOXIN ON BRICK CHEESE1

1972 ◽  
Vol 35 (10) ◽  
pp. 585-587 ◽  
Author(s):  
C. N. Shih ◽  
E. H. Marth
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Aspergillus Flavus ◽  
Aspergillus Parasiticus ◽  
Solvent System ◽  
Experimental Production ◽  
Mold Growth ◽  
Layer Chromatography ◽  
Plastic Containers ◽  
Chloroform Methanol

Brick cheese was placed in plastic containers and all surfaces except the top were sealed with wax. The top was inoculated with Aspergillus flavus or Aspergillus parasiticus and cheese was incubated in a humid chamber at 7.2, 12.8, and 23.9 C for up to 14 weeks after mold growth was evident. After incubation each cheese was cut horizontally into four layers, each approximately 1 cm thick. Each layer of cheese was extracted with a monophasic-biphasic solvent system (chloroform, methanol, and water). The extract was purified, concentrated, and aflatoxins were measured by thin-layer chromatography and fluorometry. No aflatoxins were produced by either mold at 7.2 C. At 12.8 C, A. parastticus developed aflatoxins B1 and G1 after 1 week of incubation. Aflatoxin produced by this mold persisted through 4 weeks of storage and then was not detectable. Aspergillus flavus did not form aflatoxin at 12.8 C. Both molds produced aflatoxin on cheese at 23.9 C; A. parasiticus did so after 1 week and A. flavus after 14 weeks. In some instances, aflatoxin was found in cheese 4 cm from the surface. It is reasonable to assume that cheese will not become contaminated with aflatoxin if the food is held at or below 7 C.

scholarly journals Quantitative Analysis of Sulpiride and Impurities of 2-Aminomethyl-1-Ethylpyrrolidine and Methyl-5-Sulphamoyl-2-Methoxybenzoate in Pharmaceuticals by High-Performance Thin-Layer Chromatography and Scanning Densitometry

1999 ◽  
Vol 82 (4) ◽  
pp. 825-829 ◽  
Author(s):  
Danica Agbaba ◽  
Tatjana Miljkovic ◽  
Valentina Marinkovic ◽  
Dobrila Zivanov-Stakic ◽  
Sote Vladimirov
Keyword(s):  
Quantitative Analysis ◽  
Thin Layer ◽  
High Performance ◽  
Methylene Chloride ◽  
Solvent System ◽  
Ammonia Solution ◽  
Dosage Forms ◽  
Raw Material ◽  
Layer Chromatography

Abstract A simple and reliable thin-layer chromatographic method for determining sulpiride and impurities of 2-aminomethyl-1-ethylpyrrolidine and methyl-5-sulphamoyl-2-methoxybenzoate was developed and validated. A methylene chloride–methanol–ammonia solution (25%; 18 + 2.8 + 0.4, v/v) solvent system is used for separation and quantitative evaluation of chromatograms. The chromatographic plate is first scanned at 240 nm to locate chromatographic zones corresponding to sulpiride and methyl-5-sulphamoyl-2-methoxybenzoate. Then 2-aminomethyl-1-ethylpyrrolidine is derivatized in situ with ninhydrin, and resulting colored spots are measured at 500 nm. The method is reproducible and convenient for quantitative analysis and purity control of sulpiride in its raw material and in its dosage forms.

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