Chromatographic determination of radiochemical purity

2010 ◽  
Vol 49 (02) ◽  
pp. 73-77 ◽  
Author(s):  
P. Herrling ◽  
A. Zürn ◽  
P. Anders ◽  
J. Kotzerke ◽  
G. Wunderlich
Keyword(s):  
Quality Control ◽  
Thin Layer ◽  
Glass Fibre ◽  
Radiochemical Purity ◽  
Chromatographic Determination ◽  
Acceptable Range ◽  
Mobile Phases ◽  
The Common ◽  
Layer Chromatography

SummaryThin layer chromatography is well established for quality control of radiopharmaceuticals. A convenient and widely used stationary phase are ITLC SG strips. However, the Pall Corporation stopped manufacturing of the silica gel impregnated glass fibre strips (ITLC SG). Material, Methode: As a replacement we tested silicic acid impregnated glass fibre strips from Varian (ITLC SA) and sufficient mobile phases. Results: The chromatography with these strips takes two to three times longer than with ITLC SG, but it is in an acceptable range. Only three mobile phases are necessary to test most of the common in-house made radiopharmaceuticals. Conclusion: The proposed method is suitable for routinely measuring the radiochemical purity of radiophamaceuticals.

Rapid Thin Layer Chromatographic Determination of Aflatoxin M1 in Powdered Milk

1985 ◽  
Vol 68 (5) ◽  
pp. 952-954
Author(s):  
Maria Luisa Serralheiro ◽  
Maria Lurdes Quinta
Keyword(s):  
Aqueous Solution ◽  
Carbon Tetrachloride ◽  
Thin Layer ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Methanol Solution ◽  
Aflatoxin M1 ◽  
Powdered Milk ◽  
Layer Chromatography

Abstract A method has been developed for the detection of aflatoxin Mi in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of Mi in powdered milk is 0.5 μg/ kg; recoveries of added Mj are about 83%. The limit of detection can be improved to 0.3 μg/kg if the plate is sprayed with an aqueous solution of H2S04 after development.

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.

Simultaneous Extraction and Fractionation and Thin Layer Chromatographic Determination of 14 Mycotoxins in Grains

1979 ◽  
Vol 62 (3) ◽  
pp. 573-578 ◽  
Author(s):  
Yuiko Takeda ◽  
Etsuko Isohata ◽  
Ryuji Amano ◽  
Mitsuru Uchiyama
Keyword(s):  
Thin Layer ◽  
Chromatographic Determination ◽  
Chloroform Extract ◽  
Simultaneous Extraction ◽  
Polished Rice ◽  
Rough Rice ◽  
The Individual ◽  
Layer Chromatography ◽  
Chloroform Methanol

Abstract A simple, systematic analytical method for multiple mycotoxins was developed for detecting 14 mycotoxins: aflatoxins Bl, B2, G1, and G2, sterigmatocystin, T-2 toxin, diacetoxyscirpenol, neosolaniol, fusarenon X, zearalenone, ochratoxin A, citrinin, luteoskyrin, and rugulosin. These mycotoxins were extracted with 20% H2SO4-4% KCl-acetonitrile (2+20+178), defatted with isooctane, and transferred to chloroform. The chloroform extract was cleaned up by silica gel column chromatography; the first 10 toxins were eluted with chloroform-methanol (97+3) and the remaining 4 toxins with benzene-acetone-acetic acid (75+20+5). Each fraction was analyzed by thin layer chromatography for the final determination. The method has been applied to polished rice, rough rice, corn, wheat, and peanuts as an analytical screening procedure. The detection limits in these commodities ranged from 10.0 to 800.0 μg/kg, depending on the mycotoxin, but all limits were superior to those obtained for the individual mycotoxins by using other methods.

scholarly journals Scientific-methodological approach for standardization of herbal raw materials and herbal preparations using high-performance thin-layer chromatography procedure

2021 ◽  
pp. 76-89
Author(s):  
К. О. Хохлова
Keyword(s):  
Quality Control ◽  
Thin Layer ◽  
Related Species ◽  
High Performance ◽  
Raw Materials ◽  
Methodological Approach ◽  
Herbal Drugs ◽  
Closely Related Species ◽  
Layer Chromatography

The high-performance thin-layer chromatography (HPTLC) is widely used for quality control of herbal raw materials (HRM). The purpose of this work were to define the problematic issues of quality control of herbal drugs in Ukraine and to develop a systematic scientific and methodological approach for the standardization of HRM and herbal drugs using the modern analytical technique of HPTLC: to optimize the existing and develop new methods of identification and determination of adulterations, and to develop alternative methods of quantitative determination, as well as studying of the stability. As a result of a critical evaluation of existing approaches for the standardization of HRM and herbal drugs of Ukraine’s flora, numerous problematic issues were identified, including the existence of a limited number of national monographs / national parts of monographs on the HRM of the Ukraine’s flora, which were not previously standardized by other pharmacopeias; non-consideration of Ukraine’s flora species (non-pharmacopoeial) in monographs on closely related species that introduced in the State Pharmacopoeia of Ukraine; lack of specificity of combinations of physical and chemical methods used for quality control; lack of specificity and reproducibility, the labor intensity of methods; necessity of usage of toxic solvents and precursors; use of different groups of markers and methods for the HRM and its finished product or HRM and its closely related species, etc. The proposed systematic scientific and methodological approach includes: a preliminary collection of information about the object of study, markers/groups of bioactive substances, approaches to its standardization; theoretical evaluation of existing techniques of quality control in monographs on HRM and experimental approbation using samples of domestic plants, determination of the need for optimization of existed methods by the parallel development of specific, reproducible and documented methods for identification, adulterations’ detection, quantification, and bio-detection (if necessary) by HPTLC method. The approach is illustrated with examples. The proposed approach can be used for comprehensive HPTLC analysis of domestic HRM and herbal drugs for research, prevention of adulteration, standardization of initial HRM and its finished product, pharmaceutical development, and stability studies.

scholarly journals Thin-Layer Chromatographic Determination of Monensin in Feeds: Screening Method

1998 ◽  
Vol 81 (4) ◽  
pp. 844-847 ◽  
Author(s):  
Wynne W Landgraf ◽  
P Frank Ross
Keyword(s):  
Solid Phase Extraction ◽  
Thin Layer ◽  
Solid Phase ◽  
Screening Method ◽  
Chromatographic Determination ◽  
Phase Extraction ◽  
Color Development ◽  
Layer Chromatography ◽  
Positive Results

Abstract Monensin is extracted from feed with methanol and purified by solvent-partitioning solid-phase extraction. After solvent reduction, monensin is separated by thin-layer chromatography on silica gel and visualized by color development with vanillin. No false-positive results were obtained in validation studies by submitting or peer laboratories when blank samples were analyzed. Three of 20 samples spiked with 5 ppm monensin were reported as containing no monensin. All samples spiked with 10 ppm monensin were reported positive for monensin.

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.

Collaborative Study of a Fluorometric and Thin Layer Chromatographic Determination of Aminacrine and Its Salts in Drug Preparations

1967 ◽  
Vol 50 (3) ◽  
pp. 680-682
Author(s):  
Laura A Roberts
Keyword(s):  
Standard Deviation ◽  
Thin Layer ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Assay Method ◽  
The Mean ◽  
Layer Chromatography ◽  
Mean Concentration

Abstract Eight collaborators studied a fluoromelric and thin layer chromatographic method for aminacrine and its salts in powder and cream drug preparations. Recovery of aminacrine.HCI by fluorometer in both preparations averaged 100% for powder and 102% for cream. The mean concentration of aminacrine.HCI found in the powder was 0.108% with a standard deviation of ± 0.001%. The mean concentration of aminacrine found in the cream was 0.191% with a standard deviation of ± 0.003%. Seven of the 8 collaborators successfully used thin layer chromatography to identify the aminacrine in both sample forms supplied. The assay method for aminacrine and its salts in drug preparations is recommended for adoption as official, first action

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