EUROPEAN PHARMACOPOEIA 9.0
Magnesium carbonate, heavy
ASSAY
Dissolve 0.150 g in 300 mL of water R. Carry out the
complexometric titration of magnesium {2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 14.24 mg of
C4H6Mg04.
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MAGNESIUM ASPARTATE DIHYDRATE
Magnesii aspartas dihydricus
Mg
C8H12MgN208;2H20
"02C
.  2 H20
M, 324.5
DEFINITION
Magnesium di[(S)-2-aminohydrogenobutane-l,4-dioate] dihydrate.
Content: 98.0 per cent to 102.0 per cent (anhydrous substance). CHARACTERS
Appearance: white or almost white, crystalline powder or
colourless crystals.
Solubility: freely soluble in water.
IDENTIFICATION
A. Specific optical rotation (see Tests).
B. Examine the chromatograms obtained in the test for ninhydrin-positive substances. The principal spot in the chromatogram obtained with test solution (b) is similar in position, colour and size to the principal spot in the chromatogram obtained with reference solution (a).
C. Ignite about 15 mg until a white residue is obtained. Dissolve the residue in 1 mL of dilute hydrochloric acid R, neutralise to red litmus paper R by adding dilute sodium hydroxide solution R and filter if necessary. The solution gives the reaction of magnesium (2.3.1).
TESTS
Solution S. Dissolve 2.5 g in carbon dioxide-free water R prepared from distilled water R and dilute to 100 mL with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and colourless (2.2.2, Method II).
pH (2.2.3): 6.0 to 8.0 for solution S.
Specific optical rotation (2.2.7): + 22.0 to + 24.0 (anhydrous substance).
Dissolve 0.50 g in a 515 g/L solution of hydrochloric acid R and dilute to 25.0 mL with the same acid.
Ninhydrin-positive substances. Thin-layer chromatography (2.2.27).
Test solution (a). Dissolve 0.10 g of the substance to be examined in water R and dilute to 10 mL with the same solvent.
Test solution (b). Dilute 1 mL of test solution (a) to 50 mL with water R.
Reference solution (a). Dissolve 10 mg of magnesium aspartate dihydrate CRS in water R and dilute to 50 mL with the same solvent.
Reference solution (b). Dilute 5 mL of test solution (b) to 20 mL with water R.
Reference solution (c). Dissolve 10 mg of glutamic acid CRS and 10 mg of magnesium aspartate dihydrate CRS in 2 mL of water R and dilute to 25 mL with the same solvent. Plate: TLC silica gel plate R.
Mobile phase: glacial acetic acid R, water R, butanol R
(20:20:60 V/V/V).
Application: 5 uL.
Development: over 2/3 of the plate.
Drying: in air.
Detection: spray with ninhydrin solution R and heat at 105 °C for 15 min.
System suitability: reference solution (c): the chromatogram shows 2 clearly separated principal spots. Limit:
- any impurity: any spot in the chromatogram obtained with test solution (a) is not more intense than the spot in the chromatogram obtained with reference solution (b) (0.5 per cent).
Chlorides (2.4.4): maximum 200 ppm.
Dilute 10 mL of solution S to 15 mL with water R.
Sulfates (2.4.13): maximum 500 ppm.
Dilute 12 mL of solution S to 15 mL with distilled water R.
Carry out the evaluation of the test after 30 min.
Ammonium (2.4.1): maximum 200 ppm.
50 mg complies with test B. Prepare the standard using 0.1 mL
of ammonium standard solution (100 ppm NHJ R.
Iron (2.4.9): maximum 50 ppm.
In a separating funnel, dissolve 0.20 g in 10 mL of dilute hydrochloric acid R. Shake with 3 quantities, each of 10 mL, of methyl isobutyl ketone Rl, shaking for 3 min each time. To the combined organic layers add 10 mL of water R and shake for 3 min. Use the aqueous layer.
Water (2.5.12): 10.0 per cent to 14.0 per cent, determined on 0.100 g.
Dissolve the substance in 10 mL offormamide Rl at 50 °C protected from moisture, add 10 mL of anhydrous methanol R and allow to cool. Carry out a blank determination.
ASSAY
Dissolve 0.260 g in 10 mL of water R and carry out the
complexometric titration of magnesium (2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 28.85 mg of
C8H12MgN2Os.
IMPURITIES
H NH,
H02Cv
A. (2S)-2-aminobutanedioic acid (aspartic acid).
01/2017:0043
MAGNESIUM CARBONATE, HEAVY
Magnesii subcarbonas ponderosus
DEFINITION
Hydrated basic magnesium carbonate.
Content: 40.0 per cent to 45.0 per cent, calculated as MgO
(Mr 40.30).
CHARACTERS
Appearance: white or almost white powder.
General Notices (1) apply to all monographs and other texts
2955
Magnesium carbonate, light
EUROPEAN PHARMACOPOEIA 9.0
Solubility: practically insoluble in water. It dissolves in dilute acids with effervescence.
IDENTIFICATION
A. Bulk density (2.9.34): minimum 0.25 g/mL.
B. It gives the reaction of carbonates (2.3.1).
C. Dissolve about 15 mg in 2 mL of dilute nitric acid R and neutralise with dilute sodium hydroxide solution R. The solution gives the reaction of magnesium (2.3.1).
TESTS
Solution S. Dissolve 5.0 g in 100 mL of dilute acetic acid R. When the effervescence has ceased, boil for 2 min, allow to cool and dilute to 100 mL with dilute acetic acid R. Filter, if necessary, through a previously ignited and tared porcelain or silica filter crucible of suitable porosity to give a clear filtrate.
Appearance of solution. Solution S is not more intensely coloured than reference solution B4 (2.2.2, Method II).
Soluble substances: maximum 1.0 per cent. Mix 2.00 g with 100 mL of water R and boil for 5 min. Filter whilst hot through a sintered-glass filter (40) (2.2.2), allow to cool and dilute to 100 mL with water R. Evaporate 50 mL of the filtrate to dryness and dry at 100-105 °C. The residue weighs not more than 10 mg.
Substances insoluble in acetic acid: maximum 0.05 per cent. Any residue obtained during the preparation of solution S, washed, dried, and ignited at 600 ± 50 °C, weighs not more than 2.5 mg.
Chlorides (2.4.4): maximum 700 ppm.
Dilute 1.5 mL of solution S to 15 mL with water R.
Sulfates (2.4.13): maximum 0.6 per cent.
Dilute 0.5 mL of solution S to 15 mL with distilled water R.
Arsenic (2.4.2, Method A): maximum 2 ppm, determined on 10 mL of solution S.
Calcium (2.4.3): maximum 0.75 per cent.
Dilute 2.6 mL of solution S to 150 mL with distilled water R.
15 mL of the solution complies with the test.
Iron (2.4.9): maximum 400 ppm.
Dissolve 0.1 g in 3 mL of dilute hydrochloric acid R and dilute to 10 mL with water R. Dilute 2.5 mL of the solution to 10 mL with water R.
ASSAY
Dissolve 0.150 g in a mixture of 2 mL of dilute hydrochloric acid R and 20 mL of water R. Carry out the complexometric titration of magnesium (2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 4.030 mg of MgO.
FUNCTIONALITY-RELATED CHARACTERISTICS This section provides information on characteristics that are recognised as being relevant control parameters for one or more functions of the substance when used as an excipient (see chapter 5.15). Some of the characteristics described in the Functionality-related characteristics section may also be present in the mandatory part of the monograph since they also represent mandatory quality criteria. In such cases, a cross-reference to the tests described in the mandatory part is included in the Functionality-related characteristics section. Control of the characteristics can contribute to the quality of a medicinal product by improving the consistency of the manufacturing process and the performance of the medicinal product during use. Where control methods are cited, they are recognised as being suitable for the purpose, but other methods can also be used. Wherever results for a particular characteristic are reported, the control method must be indicated. The following characteristics may be relevant for heavy magnesium carbonate used as filler in tablets.
Particle-size distribution (2.9.31 or 2.9.38). Bulk and tapped density (2.9.34).
01/2017:0042
MAGNESIUM CARBONATE, LIGHT
Magnesii subcarbonas levis
DEFINITION
Hydrated basic magnesium carbonate.
Content: 40.0 per cent to 45.0 per cent, calculated as MgO
(Mr 40.30).
CHARACTERS
Appearance: white or almost white powder.
Solubility: practically insoluble in water. It dissolves in dilute
acids with effervescence.
IDENTIFICATION
A. Bulk density (2.9.34): maximum 0.15 g/mL.
B. It gives the reaction of carbonates (2.3.1).
C. Dissolve about 15 mg in 2 mL of dilute nitric acid R and neutralise with dilute sodium hydroxide solution R. The solution gives the reaction of magnesium (2.3.1).
TESTS
Solution S. Dissolve 5.0 g in 100 mL of dilute acetic acid R. When the effervescence has ceased, boil for 2 min, allow to cool and dilute to 100 mL with dilute acetic acid R. Filter, if necessary, through a previously ignited and tared porcelain or silica filter crucible of suitable porosity to give a clear filtrate.
Appearance of solution. Solution S is not more intensely coloured than reference solution B4 (2.2.2, Method II).
Soluble substances: maximum 1.0 per cent. Mix 2.00 g with 100 mL of water R and boil for 5 min. Filter whilst hot through a sintered-glass filter (40) (2.1.2), allow to cool and dilute to 100 mL with water R. Evaporate 50 mL of the filtrate to dryness and dry at 100-105 °C. The residue weighs a maximum of 10 mg.
Substances insoluble in acetic acid: maximum 0.05 per cent. Any residue obtained during the preparation of solution S, washed, dried and ignited at 600 ± 50 °C, weighs a maximum of 2.5 mg.
Chlorides (2.4.4): maximum 700 ppm.
Dilute 1.5 mL of solution S to 15 mL with water R.
Sulfates (2.4.13): maximum 0.3 per cent.
Dilute 1 mL of solution S to 15 mL with distilled water R.
Arsenic (2.4.2, Method A): maximum 2 ppm, determined on 10 mL of solution S.
Calcium (2.4.3): maximum 0.75 per cent.
Dilute 2.6 mL of solution S to 150 mL with distilled water R.
15 mL of the solution complies with the test.
Iron (2.4.9): maximum 400 ppm.
Dissolve 0.1 g in 3 mL of dilute hydrochloric acid R and dilute to 10 mL with water R. Dilute 2.5 mL of this solution to 10 mL with water R.
ASSAY
Dissolve 0.150 g in a mixture of 2 mL of dilute hydrochloric acid R and 20 mL of water R. Carry out the complexometric titration of magnesium (2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 4.030 mg of MgO.
2956
See the information section on general monographs (cover pages)