This document provides information on aminoglutethimide, including its definition, characteristics, identification tests, purity tests, and assay method. Some key details include:
- It defines aminoglutethimide as (3RS)-3-(4-aminophenyl)-3-ethylpiperidine-2,6-dione with a content of 98.0 to 101.5% of the dried substance.
- It is described as a white or slightly yellow, crystalline powder that is practically insoluble in water but freely soluble in acetone and soluble in methanol.
- Identification tests involve melting point determination, infrared spectroscopy, and thin-layer chromatography.
- Purity tests
This document provides information on aminoglutethimide, including its definition, characteristics, identification tests, purity tests, and assay method. Some key details include:
- It defines aminoglutethimide as (3RS)-3-(4-aminophenyl)-3-ethylpiperidine-2,6-dione with a content of 98.0 to 101.5% of the dried substance.
- It is described as a white or slightly yellow, crystalline powder that is practically insoluble in water but freely soluble in acetone and soluble in methanol.
- Identification tests involve melting point determination, infrared spectroscopy, and thin-layer chromatography.
- Purity tests
This document provides information on aminoglutethimide, including its definition, characteristics, identification tests, purity tests, and assay method. Some key details include:
- It defines aminoglutethimide as (3RS)-3-(4-aminophenyl)-3-ethylpiperidine-2,6-dione with a content of 98.0 to 101.5% of the dried substance.
- It is described as a white or slightly yellow, crystalline powder that is practically insoluble in water but freely soluble in acetone and soluble in methanol.
- Identification tests involve melting point determination, infrared spectroscopy, and thin-layer chromatography.
- Purity tests
01/2017:0874 Test solution (b). Dilute 1 mL of test solution (a) to 50 mL
with water R. Reference solution (a). Dissolve 10 mg of aminocaproic acid CRS in water R and dilute to 50 mL with the same solvent. Reference solution (b). Dilute 5 mL of test solution (b) to AMINOCAPROIC ACID 20 mL with water R. Reference solution (c). Dissolve 10 mg of aminocaproic Acidum aminocaproicum acid CRS and 10 mg of leucine CRS in water R and dilute to 25 mL with the same solvent. Apply separately to the plate 5 μL of each solution. Allow the plate to dry in air. Develop over a path of 15 cm using C6H13NO2 Mr 131.2 a mixture of 20 volumes of glacial acetic acid R, 20 volumes [60-32-2] of water R and 60 volumes of butanol R. Dry the plate in a current of warm air. Spray with ninhydrin solution R and heat DEFINITION at 100 °C to 105 °C for 15 min. Any spot in the chromatogram Aminocaproic acid contains not less than 98.5 per cent and not obtained with the test solution (a), apart from the principal more than the equivalent of 101.0 per cent of 6-aminohexanoic spot, is not more intense than the spot in the chromatogram acid, calculated with reference to the dried substance. obtained with reference solution (b) (0.5 per cent). The test CHARACTERS is not valid unless the chromatogram obtained with reference solution (c) shows two clearly separated principal spots. A white or almost white, crystalline powder or colourless crystals, freely soluble in water, slightly soluble in alcohol. Loss on drying (2.2.32). Not more than 0.5 per cent, determined on 1.000 g by drying in an oven at 105 °C. It melts at about 205 °C with decomposition. Sulfated ash (2.4.14). Not more than 0.1 per cent, determined IDENTIFICATION on 1.0 g. First identification : A. ASSAY Second identification : B, C, D. Dissolve 0.100 g in 20 mL of anhydrous acetic acid R. A. Examine by infrared absorption spectrophotometry Using 0.1 mL of crystal violet solution R as indicator, titrate (2.2.24), comparing with the spectrum obtained with with 0.1 M perchloric acid until the colour changes from aminocaproic acid CRS. Examine the substances prepared bluish-violet to bluish-green. as discs. 1 mL of 0.1 M perchloric acid is equivalent to 13.12 mg of B. Examine the chromatograms obtained in the test for C6H13NO2. ninhydrin-positive substances. The principal spot in the chromatogram obtained with the test solution (b) is similar 01/2017:1291 in position, colour and size to the principal spot in the chromatogram obtained with reference solution (a). C. Dissolve 0.5 g in 4 mL of a mixture of equal volumes of dilute hydrochloric acid R and water R. Evaporate to dryness by heating on a water-bath. Dry the residue in a desiccator. Dissolve the residue in about 2 mL of boiling ethanol R. AMINOGLUTETHIMIDE Allow to cool and maintain at 4 °C to 8 °C for 3 h. Filter under reduced pressure. The residue washed with about Aminoglutethimidum 10 mL of acetone R and dried at 60 °C for 30 min, melts (2.2.14) at 131 °C to 133 °C. D. Dissolve about 5 mg in 0.5 mL of distilled water R. Add 3 mL of dimethylformamide R and 2 mL of ascorbic acid solution R. Heat on a water-bath. An orange colour develops. C13H16N2O2 Mr 232.3 TESTS [125-84-8] Solution S. dissolve 10.0 g in carbon dioxide-free water R and DEFINITION dilute to 50.0 mL with the same solvent. (3RS)-3-(4-Aminophenyl)-3-ethylpiperidine-2,6-dione. Appearance of solution. Solution S is colourless (2.2.2, Method II) and remains clear (2.2.1) on standing for 24 h. Content : 98.0 per cent to 101.5 per cent (dried substance). pH (2.2.3). The pH of solution S is 7.5 to 8.0. CHARACTERS Absorbance (2.2.25). Appearance : white or slightly yellow, crystalline powder. A. The absorbance of solution S at 287 nm is not more Solubility : practically insoluble in water, freely soluble in than 0.10 and at 450 nm is not more than 0.03. acetone, soluble in methanol. B. Place 2.0 g in an even layer in a shallow dish 9 cm in IDENTIFICATION diameter, cover and allow to stand at 98 °C to 102 °C for First identification : B. 72 h. Dissolve in water R and dilute to 10.0 mL with the same solvent. The absorbance of the solution at 287 nm is Second identification : A, C. not more than 0.15 and at 450 nm is not more than 0.03. A. Melting point (2.2.14) : 150 °C to 154 °C. Ninhydrin-positive substances. Examine by thin-layer B. Infrared absorption spectrophotometry (2.2.24). chromatography (2.2.27), using a suitable silica gel as the Comparison : aminoglutethimide CRS. coating substance. C. Thin-layer chromatography (2.2.27). Test solution (a). Dissolve 0.10 g of the substance to be Test solution. Dissolve 25 mg of the substance to be examined in water R and dilute to 10 mL with the same examined in acetone R and dilute to 5 mL with the same solvent. solvent.
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