Quality control methods for
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- Silica gel H
Silica gel GF
254 Description. A fine, white, homogeneous powder with an average particle size of between 10 and 40 µm containing about 130 g of calcium sulfate, hemihydrate per kg and about 150 g of a fluorescent indicator per kg with an optimal intensity at 254 nm. Content of calcium sulfate. Place about 0.25 g, accurately weighed, in a flask with a ground-glass stopper, add 3 ml of hydrochloric acid (~70 g/l) TS and 100 ml of water and shake vigorously for 30 minutes. Filter through a sintered-glass filter and wash the residue. Using the combined filtrate and washings, carry out the assay for calcium by complexometry (The international pharmacopoeia, Vol. 1, page 128). Each ml of disodium edetate (0.05 mol/l) VS is equivalent to 7.26 mg of CaSO 4 ,1/2H 2 O (M r 145.1). pH. Shake 1 g with 10 ml of carbon-dioxide-free water R for 5 minutes. Measure the pH potentiometrically (The international pharmacopoeia, Vol. 1, page 96); pH is about 7. Quality control methods for medicinal plant materials Preparation. Suspend 30g in 60 ml of water, shaking vigorously for 30 seconds. Carefully coat the cleaned plates with a layer 0.25 mm thick using a spreading device. Allow the coated plates to dry in air. Separating power. Apply separately to the adsorbent layer 10 µl of 0.10 mg/ml solutions containing respectively indophenol blue R, sudan red G R and dimethyl yellow R in toluene R. Develop the plate with the same solvent over a distance of 10 cm. The chromatogram shows three clearly separated spots, the spot of indophenol blue near the point of application, that of dimethyl yellow in the middle of the chromatogram, and that of sudan red G between the two. Fluorescence. Prepare a 1.0 mg/ml solution of benzoic acid R in a mixture of 9 volumes of 2-propanol R and 1 volume of formic acid (~1080g/l) TS. Apply to the adsorbent layer at 10 points of application, increasing the quantities of the solution from 1 µl to 10 µl. Develop the chromatogram using a mixture of 9 volumes of 2-propanol R and 1 volume of formic acid (~1080 g/l) TS. Allow the solvents to evaporate and examine the chromatogram in ultraviolet light at 254 nm. The benzoic acid appears as dark spots on a fluorescent background in the upper third of the chromatogram for amounts of 2 µg and more. Silica gel H Description. A fine, white, homogeneous powder with an average particle size of between 10 and 44 µm. pH. Shake 1 g with 10 ml of carbon-dioxide-free water R for 5 minutes. Measure the pH potentiometrically (The international pharmacopoeia, Vol. 1, page 96); pH is about 7. Preparation. Suspend 30g in 60 ml of water, shaking vigorously for 30 seconds. Carefully coat the cleaned plates with a layer 0.25 mm thick using a spreading device. Allow the coated plates to dry in air. Separating power. Apply separately to the adsorbent layer 10 µl of 0.10 mg/ml solutions containing respectively indophenol blue R, sudan red G R and dimethyl yellow R in toluene R. Develop the plate with the same solvent over a distance of 10 cm. The chromatogram shows three clearly separated spots, the spot of indophenol blue near the point of application, that of dimethyl yellow in the middle of the chromatogram, and that of sudan red G between the two. Download 1.63 Mb. Do'stlaringiz bilan baham: |
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