Magnesium citrate nonahydrate EUROPEAN PHARMACOPOEIA 8.0

thanthatofastandardpreparedatthesametimeandinthe Oxalates: maximum 280 ppm. same manner using 4 mL of a 50 mg/L solution of oxalic Dissolve 0.50 g in a mixture of 3 mL of hydrochloric acid R and acid R. 4mLofwater R and add 1 g of activated zinc R.Allowtostand Sulfates (2.4.13): maximum 0.2percent. for 5 min. Transfer the liquid to a tube containing 0.25 mL of Dilute 3.0 mL of solution S to 15 mL with distilled water R. a 10 g/L solution of phenylhydrazine hydrochloride R.Heat Calcium to boiling. Cool rapidly, transfer to a graduated cylinder and (2.4.3): maximum 0.2 percent. add an equal volume of hydrochloric acid R and 0.25 mL of To a mixture of 2 mL of solution S and 8 mL of distilled potassium ferricyanide solution R.Shakeandallowtostandfor water R, add about 0.2 mL of ammonia R and dilute to 15 mL 30 min. Any pink colour in the solution is not more intense with distilled water R. than that of a standard prepared at the same time and in the Iron (2.4.9): maximum 100 ppm. same manner using 4 mL of a 50 mg/L solution of oxalic Dilute 4.0 mL of solution S to 10 mL with distilled water R. acid R. Sulfates Heavy metals (2.4.8): maximum 10 ppm. (2.4.13): maximum 0.2percent. Dissolve 5.0 g in 15 mL of dilute hydrochloric acid R with Dilute 3.0 mL of solution S to 15 mL with distilled water R. heating. Adjust to pH 3.5 with ammonia R and dilute to Calcium (2.4.3): maximum 0.2 percent. 50 mL with distilled water R. 12 mL of the solution complies To a mixture of 2 mL of solution S and 8 mL of distilled with test A. Prepare the reference solution using lead standard water R,addabout0.2mLofammonia R and dilute to 15 mL solution (1 ppm Pb) R. with distilled water R. Loss on drying (2.2.32): 29.0 per centto 36.0 per cent, Iron (2.4.9): maximum 100 ppm. determined on 1.000 g by drying in an oven at 180 ± 10 °C Dilute 4.0 mL of solution S to 10 mL with distilled water R. for 5 h. Heavy metals (2.4.8): maximum 10 ppm. ASSAY Dissolve 5.0 g in 15 mL of dilute hydrochloric acid R with Dissolve 0.200 g in 5 mL of dilute hydrochloric acid R with heating. Adjust to pH 3.5 with ammonia R and dilute to heating. Cool and add 50 mL of water R.AdjusttopH7.0 50 mL with distilled water R. 12 mL of the solution complies with ammonia R. Carry out the complexometric titration of with test A. Prepare the reference solution using lead standard magnesium (2.5.11). solution (1 ppm Pb) R. 1mLof0.1 M sodium edetate is equivalent to 2.431 mg of Mg. Loss on drying (2.2.32): 24.0 to 28.0 per cent, determined on 1.000 g by drying in an oven at 180 ± 10 °C for 5 h. 01/2010:2402 ASSAY MAGNESIUM CITRATE Dissolve 0.200 g in 5 mL of dilute hydrochloric acid R with heating. Cool and add 50 mL of water R.AdjusttopH7.0 NONAHYDRATE with ammonia R. Carry out the complexometric titration of magnesium (2.5.11). Magnesii citras nonahydricus 1mLof0.1 M sodium edetate is equivalent to 2.431 mg of Mg.

04/2008:2161 MAGNESIUM GLUCONATE

Mg3(C6H5O7)2,9H2O Mr 613 [153531-96-5] Magnesii gluconas DEFINITION Trimagnesium bis(2-hydroxypropane-1,2,3-tricarboxylate) nonahydrate. Content: 15.0 per cent to 16.5 per cent of Mg (dried substance). CHARACTERS Appearance: white or almost white, fine powder. C12H22MgO14,xH2O Mr 414.6 (anhydrous substance) Solubility: sparingly soluble in water, practically insoluble in DEFINITION ethanol (96 per cent). It dissolves in dilute hydrochloric acid. Anhydrous or hydrated magnesium D-gluconate. IDENTIFICATION Content: 98.0 per cent to 102.0 per cent (anhydrous substance). A. It gives the reaction of citrates (2.3.1). CHARACTERS B. It gives the reaction of magnesium (2.3.1). Appearance: white or almost white, amorphous, hygroscopic, C. Loss on drying (see Tests). crystalline or granular powder. TESTS Solubility: freely soluble in water, slightly soluble in ethanol (96 per cent), very slightly soluble in methylene chloride. Solution S. Dissolve 2.5 g in 15 mL of dilute hydrochloric acid R with heating. Cool and dilute to 100 mL with distilled IDENTIFICATION water R. A. Thin-layer chromatography (2.2.27). Appearance of solution. Solution S is clear (2.2.1)and Test solution.Dissolve20mgofthesubstancetobe not more intensely coloured than reference solution BY6 examined in 1 mL of water R. (2.2.2, Method II). Reference solution.Dissolve20mgofcalcium gluconate CRS pH (2.2.3): 6.0 to8.5. in 1 mL of water R, heating if necessary in a water-bath Disperse 5.0 g in carbon dioxide-free water R and dilute to at 60 °C. 100 mL with the same solvent. Centrifuge and measure the Plate: TLC silica gel plate R (5-40 μm) [or TLC silica gel pH of the clear supernatant. plate R (2-10 μm)].

2674 See the information section on general monographs (cover pages) EUROPEAN PHARMACOPOEIA 8.0 Magnesium glycerophosphate

Mobile phase: concentrated ammonia R, ethyl acetate R, DEFINITION water R, ethanol (96 per cent) R (10:10:30:50 V/V/V/V). Mixture, in variable proportions, of magnesium Application:1μL. salts of (RS)-2,3-dihydroxypropyl phosphate and Development:over3/4oftheplate. 2-hydroxy-1-(hydroxymethyl)ethyl phosphate, which may be Drying: at 100-105 °C for 20 min, then allow to cool to hydrated. room temperature. Content: 11.0 per cent to 12.5 per cent of Mg (dried substance). Detection: spray with a solution containing 25 g/L of CHARACTERS ammonium molybdate R and 10 g/L of cerium sulfate R in dilute sulfuric acid R,thenheatat100-105°Cforabout Appearance: white or almost white powder, hygroscopic. 10 min. Solubility: practically insoluble in ethanol (96 per cent). It Results: the principal spot in the chromatogram obtained dissolves in dilute solutions of acids. with the test solution is similar in position, colour and size IDENTIFICATION to the principal spot in the chromatogram obtained with the reference solution. A. Mix 1 g with 1 g of potassium hydrogen sulfate R in atesttubefittedwithaglasstube.Heatstronglyand B. To 10 mL of solution S (see Tests) add 3 mL of ammonium direct the white vapour towards a piece of filter paper chloride solution R. A slight opalescence may be observed. impregnated with a freshly prepared 10 g/L solution of Add 10 mL of disodium hydrogen phosphate solution R.A sodium nitroprusside R.Thefilterpaperdevelopsablue white precipitate is formed that does not dissolve upon the colour in contact with piperidine R. addition of 2 mL of dilute ammonia R1. B. Ignite 0.1 g in a crucible. Take up the residue with 5 mL of TESTS nitric acid R and heat on a water-bath for 1 min. Filter. The Solution S.Dissolve1.0ginwater R and dilute to 50 mL with filtrate gives reaction (b) of phosphates (2.3.1). the same solvent. C. It gives the reaction of magnesium (2.3.1). Appearance of solution . Solution S is clear (2.2.1) and not TESTS more intensely coloured than reference solution Y (2.2.2, 7 Solution S Method II). .Dissolve2.5gincarbon dioxide-free water R Sucrose and reducing sugars prepared from distilled water R and dilute to 50 mL with the .Dissolve0.5ginamixtureof same solvent. 2mLofhydrochloric acid R1 and 10 mL of water R. Boil for Appearance of solution 5 min, allow to cool, add 10 mL of sodium carbonate solution R . Solution S is not more opalescent andallowtostandfor10min.Diluteto25mLwithwater R than reference suspension III (2.2.1). and filter. To 5 mL of the filtrate add 2 mL of cupri-tartaric Acidity.Dissolve1.0gin100mLofcarbon dioxide-free solution R and boil for 1 min. Allow to stand for 2 min. No water R.Add0.1mLofphenolphthalein solution R.Notmore red precipitate is formed. than 1.5 mL of 0.1 M sodium hydroxide is required to change Chlorides (2.4.4): maximum 500 ppm. the colour of the indicator. Dilute 5 mL of solution S to 15 mL with water R. Glycerol and ethanol (96 per cent)-soluble substances: Sulfates (2.4.13): maximum 500 ppm. maximum 1.5 per cent. Dissolve2.0ginamixtureof10mLofacetic acid R and 90 mL Shake 1.0 g with 25 mL of ethanol (96 per cent) R for 2 min. of distilled water R. Filter and wash the residue with 5 mL of ethanol (96 per cent) R. Combine the filtrate and the washings, evaporate to Heavy metals (2.4.8): maximum 10 ppm. dryness on a water-bath and dry the residue at 70 °C for 1 h. Dissolve 2.0 g in 20 mL of water R.12mLofthesolution The residue weighs a maximum of 15 mg. complies with test A. Prepare the reference solution using lead Chlorides (2.4.4): maximum 0.15 per cent. standard solution (1 ppm Pb) R. Water Dissolve 1.0 g in water R and dilute to 100 mL with the same (2.5.32): maximum 12.0 per cent, determined on 80 mg. solvent. Dilute 3.5 mL of this solution to 15 mL with water R. Microbial contamination . Total viable aerobic count (2.6.12) Phosphates (2.4.11): maximum0.5percent. not more than 103 micro-organisms per gram, determined by plate count. Dilute4mLofsolutionSto100mLwithwater R.Dilute1mL of this solution to 100 mL with water R. ASSAY Sulfates (2.4.13): maximum 0.1percent. Dissolve 0.350 g in 100 mL of water R and carry out the Dilute 3 mL of solution S to 15 mL with distilled water R. complexometric titration of magnesium (2.5.11). Iron (2.4.9): maximum 150 ppm. 1mLof0.1 M sodium edetate is equivalent to 41.46 mg of C H MgO . Dissolve 67 mg in water R and dilute to 10 mL with the same 12 22 14 solvent. STORAGE Heavy metals (2.4.8): maximum 20 ppm. In an airtight container. To 20 mL of solution S add 15 mL of hydrochloric acid R and 01/2008:1446 shake with 25 mL of methyl isobutyl ketone R for 2 min. Allow corrected 6.0 to stand, then separate and evaporate the aqueous layer to dryness. Dissolve the residue in 2.5 mL of acetic acid R and MAGNESIUM GLYCEROPHOSPHATE dilute to 20 mL with water R.12mLofthesolutioncomplies with test A. Prepare the reference solution using lead standard solution (1 ppm Pb) R. Magnesii glycerophosphas Loss on drying (2.2.32): maximum 12.0 per cent, determined on1.000gbydryinginanovenat150°Cfor4h. ASSAY Dissolve 0.200 g in 40 mL of water R.Carryoutthe complexometric titration of magnesium (2.5.11).

C3H7MgO6P Mr 194.4 1mLof0.1 M sodium edetate is equivalent to 2.431 mg of Mg.

General Notices (1) apply to all monographs and other texts 2675