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0 Magnesium stearate
General Notices (1) apply to all monographs and other texts 3163
Magnesium stearate EUROPEAN PHARMACOPOEIA 10.0
Operating conditions : use the temperature programme Test solution. Use the solution described in the test for
recommended for cadmium by the GFAA spectrometer cadmium.
manufacturer. An example of temperature parameters for Reference solution. Prepare a solution of 0.050 μg/mL of Ni by
GFAA analysis of cadmium is shown below. suitable dilutions of a 0.2477 μg/mL solution of nickel nitrate
Stage Final temperature Ramp time Hold time hexahydrate R in the blank solution.
(°C) (s) (s) Prepare mixtures of the test solution, the reference solution
Drying 110 10 20 and the blank solution in the following proportions :
(1.0:0:1.0 V/V/V), (1.0:0.5:0.5 V/V/V), (1.0:1.0:0 V/V/V). To
Ashing 600 10 30 each mixture add 50 μL of matrix modifier solution and mix.
Atomisation 1800 0 5 These reference solutions contain respectively 0 μg, 0.0125 μg
and 0.025 μg of nickel per millilitre from the reference
Lead : maximum 10 ppm. solution.
Atomic absorption spectrometry (2.2.23, Method II). Source : nickel hollow-cathode lamp.
For the preparation of all aqueous solutions and for the rinsing Wavelength : 232.0 nm.
of glassware before use, employ water that has been passed Atomisation device : furnace.
through a strong-acid, strong-base, mixed-bed ion-exchange Platform : pyrolytically coated with integrated tube.
resin before use. Select all reagents to have as low a content of Operating conditions : use the temperature programme
cadmium, lead and nickel as practicable and store all reagent recommended for nickel by the GFAA spectrometer
solutions in containers of borosilicate glass. Clean glassware manufacturer. An example of temperature parameters for
before use by soaking in a warm 773 g/L solution of nitric GFAA analysis of nickel is shown below.
acid R for 30 min and by rinsing with deionised water.
Stage Final temperature Ramp time Hold time
Blank solution. Use the solution described in the test for
(°C) (s) (s)
cadmium.
Drying 110 10 20
Modifier solution. Use the solution described in the test for
cadmium. Ashing 1000 20 30
Test solution. Use the solution described in the test for Atomisation 2300 0 5
cadmium.
Reference solution. Prepare a solution of 0.100 μg/mL of Pb by Loss on drying (2.2.32) : maximum 6.0 per cent, determined
suitable dilutions of lead standard solution (100 ppm Pb) R on 1.000 g by drying in an oven at 105 °C.
with the blank solution. ♦Microbial contamination.
Prepare mixtures of the test solution, the reference solution TAMC : acceptance criterion 103 CFU/g (2.6.12).
and the blank solution in the following proportions : TYMC : acceptance criterion 102 CFU/g (2.6.12).
(1.0:0:1.0 V/V/V), (1.0:0.5:0.5 V/V/V), (1.0:1.0:0 V/V/V). To
Absence of Escherichia coli (2.6.13).
each mixture add 50 μL of modifier solution and mix. These
solutions contain respectively 0 μg, 0.025 μg and 0.05 μg of Absence of Salmonella (2.6.13).♦
lead per millilitre from the reference solution. ASSAY
Source : lead hollow-cathode lamp.
Magnesium. To 0.500 g in a 250 mL conical flask add
Wavelength : 283.3 nm. 50 mL of a mixture of equal volumes of anhydrous ethanol R
Atomisation device : furnace. and butanol R, 5 mL of concentrated ammonia R, 3 mL of
Platform : pyrolytically coated with integrated tube. ammonium chloride buffer solution pH 10.0 R, 30.0 mL
of 0.1 M sodium edetate and 15 mg of mordant black 11
Operating conditions : use the temperature programme triturate R. Heat at 45-50 °C until the solution is clear and
recommended for lead by the GFAA spectrometer titrate with 0.1 M zinc sulfate until the colour changes from
manufacturer. An example of temperature parameters for blue to violet. Carry out a blank titration.
GFAA analysis of lead is shown below.
1 mL of 0.1 M sodium edetate is equivalent to 2.431 mg of Mg.
Stage Final temperature Ramp time Hold time Stearic acid and palmitic acid. Gas chromatography (2.2.28) :
(°C) (s) (s) use the normalisation procedure.
Drying 110 10 20
Test solution. In a conical flask fitted with a reflux condenser,
Ashing 450 10 30 dissolve 0.10 g of the substance to be examined in 5 mL of
Atomisation 2000 0 5
boron trifluoride-methanol solution R. Boil under a reflux
condenser for 10 min. Add 4 mL of heptane R through
Nickel : maximum 5 ppm. the condenser and boil again under a reflux condenser for
10 min. Allow to cool. Add 20 mL of saturated sodium
Atomic absorption spectrometry (2.2.23, Method II). chloride solution R. Shake and allow the layers to separate.
For the preparation of all aqueous solutions and for the rinsing Dry the organic layer over 0.1 g of anhydrous sodium sulfate R
of glassware before use, employ water that has been passed (previously washed with heptane R). Dilute 1.0 mL of the
through a strong-acid, strong-base, mixed-bed ion-exchange solution to 10.0 mL with heptane R.
resin before use. Select all reagents to have as low a content of Reference solution. Prepare the reference solution in the same
cadmium, lead and nickel as practicable and store all reagent manner as the test solution using 50.0 mg of palmitic acid CRS
solutions in containers of borosilicate glass. Clean glassware and 50.0 mg of stearic acid CRS instead of the substance to
before use by soaking in a warm 773 g/L solution of nitric be examined.
acid R for 30 min and by rinsing with deionised water. Column :
Blank solution. Use the solution described in the test for – material : fused silica ;
cadmium.
– size : l = 30 m, Ø = 0.32 mm ;
Modifier solution. Dissolve 20 g of ammonium dihydrogen
– stationary phase : macrogol 20 000 R (film thickness 0.5 μm).
phosphate R in water R and dilute to 100 mL with the same
solvent. Alternatively, use an appropriate matrix modifier as Carrier gas : helium for chromatography R.
recommended by the GFAA spectrometer manufacturer. Flow rate : 2.4 mL/min.
DEFINITION TESTS
Content : 99.0 per cent to 100.5 per cent (dried substance). Solution S. To 2.0 g add a mixture of 4 mL of nitric acid R
and 4 mL of distilled water R. Heat to boiling with frequent
CHARACTERS shaking. Add 12 mL of distilled water R and allow to cool.
Appearance : white or almost white, crystalline powder or Filter or centrifuge to obtain a clear solution and dilute to
brilliant, colourless crystals. 20 mL with distilled water R.
General Notices (1) apply to all monographs and other texts 3165