Simple, Rapid Cleanup Method for Analysis of Aflatoxins and Comparison with Various Methods

1985 ◽  
Vol 68 (3) ◽  
pp. 458-461 ◽  
Author(s):  
Hisashi Kamimura ◽  
Motohiro Nishijima ◽  
Kazuo Yasuda ◽  
Hirofumi Ushiyama ◽  
Setsuko Tabata ◽  
...  
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Rapid Determination ◽  
Hptlc Plate ◽  
Simple Method ◽  
Florisil Column ◽  
Chromatographic Procedure ◽  
Test Materials ◽  
Column Chromatographic

Abstract A method is described for simple and rapid determination of aflatoxins in corn, buckwheat, peanuts, and cheese. Aflatoxins were extracted with chloroform-water and were purified by a Florisil column chromatographic procedure. Column eluates were concentrated and spotted on a high performance thin layer chromatographic (HPTLC) plate, which was then developed in chloroform-acetone (9 + 1) and/or ethermethanol- water (94 + 4.5 + 1.5)orchloroform-isopropanol-acetone (85 + 5 + 10). Each aflatoxin was quantitated by densitometry. The minimum detectable aflatoxin concentrations (μg/kg) in various test materials were 0.2, B1; 0.1, B2; 0.2, G1; 0.1, G2; and 0.1,M1.Recoveries of the aflatoxins added to corn, peanut, and cheese samples at 10-30 μg/kg were > 69% (aflatoxin G2) and averaged 91%, B1; 89%, B2; 91%, G1; 78%, G2; and 92%, M1. The simple method described was compared with the AOAC CB method, AOAC BF method, and AOAC milk and cheese method. These methods were applied to corn, peanut, and cheese composites spiked with known amounts of aflatoxins, and to naturally contaminated buckwheat and cheese. Recoveries were much lower for the BF method compared with our simple method and the CB method.

scholarly journals NOVEL HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHIC METHOD FOR SIMPLE, ECONOMICAL, AND RAPID DETERMINATION OF FENOFIBRATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (5) ◽  
pp. 147
Author(s):  
Rani S Potawale ◽  
Tabassume I Hangad
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Regression Coefficient ◽  
Rapid Determination ◽  
High Sensitivity ◽  
Pharmaceutical Dosage Form ◽  
Densitometric Detection ◽  
Hptlc Method

 Objective: A simple, novel, sensitive, and rapid high-performance thin-layer chromatographic (HPTLC) method has been developed and validated for quantitative determination of fenofibrate in bulk and formulations.Methods: The chromatographic development was carried out on HPTLC plates precoated with silica gel 60 F254 using a single solvent dichloromethane as a simple mobile phase. Densitometric detection was carried out at 292 nm.Results: Rf value of drug was found to be 0.33±0.02. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 20–400° ng band−1° with a regression coefficient of 0.999. The method has proved high sensitivity and specificity.Conclusion: Proposed densitometric method was found to be new, simple, and economic for routine quantification of fenofibrate in bulk and pharmaceutical formulation.

scholarly journals Simplified two-step column-chromatographic determination of taurine in urine.

1978 ◽  
Vol 24 (2) ◽  
pp. 321-325 ◽  
Author(s):  
M A Anzano ◽  
J O Naewbanij ◽  
A J Lamb
Keyword(s):  
Present Method ◽  
Exchange Resin ◽  
Rapid Determination ◽  
Cation Exchange Resin ◽  
Chromatographic Determination ◽  
Cysteic Acid ◽  
Chromatographic Procedure ◽  
Acidic Compounds ◽  
Column Chromatographic

Abstract A two-step column-chromatographic procedure for accurate and rapid determination of taurine in urine is described. Sulfosalicyclic-acid deproteinized samples are chromatographed on a 0.9 X 10 cm column of cation-exchange resin (AG 50W-XB), with use of a pH 2.2 sodium citrate eluting buffer such that taurine and the more highly acidic compounds in urine are eluted in the void volume, and then on a 0.9 X 8 cm column of anion-exchange resin (AG 2-X8), from which taurine is preferentially eluted with 1 mol/liter acetic acid. The color developed with ninhydrin is directly proportional to taurine amounts as low as 0.01 mumol/sample. The method is highly reproducible, with analytical recoveries greater than 95%. The presence of 333 mumol of urea and 1 mumol of cysteic acid did not interfere in the analysis. When a mixture of C14-labeled amino acids other than taurine were co-chromatographed with taurine, less than 2% of the total counts loaded were located in the taurine fraction. Values for urinary taurine excretion by rats according to the present method agreed well with values obtained with an automated amino acid analyzer. Advantages of the present method for the determination of taurine are discussed.

COMPARISON OF VARIOUS METHODS FOR THE CHEMICAL ASSAY OF CORTICOIDS IN URINE

1955 ◽  
Vol 18 (4) ◽  
pp. 374-378
Author(s):  
Mogens Sprechler
Keyword(s):  
Calibration Curve ◽  
Periodic Acid ◽  
Reducing Power ◽  
Standard Technique ◽  
Phosphomolybdic Acid ◽  
Florisil Column ◽  
Chemical Assay ◽  
Chromatographic Procedure ◽  
Acid Reagent

SUMMARY Since 1949 about 10,000 urinary corticoid analyses have been performed routinely in our laboratory. The method used for this purpose was described in 1950 (Sprechler). We determine the corticoids which can be extracted from the urine with chloroform immediately after acidification to pH 1. The extract is washed with sodium hydroxide and water, a Girard separation is performed, and finally the reducing power of the ketonic fraction is measured by means of the phosphomolybdic acid reagent reaction. During the last few years two other chemical reactions have been used for comparison: The formaldehyde and the Porter-Silber method. After a thorough examination of the above methods a standard technique was followed. In the formaldehyde method a microdiffusion in a Conway unit was used instead of distillation of the formaldehyde following the oxidation with periodic acid. The calibration curve was corrected for loss of material by taking the standard doses of DOC through all the procedures of the method. A micromodification of the Porter-Silber method was chosen. Furthermore attempts were made to determine how specific the chromatographic procedure is in the determination of steroids in urinary extracts. For this purpose the Florisil column was used, and the technique described by Nelson & Samuels was followed. Finally we have investigated the glucuronide-bound corticoids in urine in a smaller series of objects.

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