Packaging and storage—
Preserve in tight, light-resistant containers.
Labeling* —
The label states that the product is Oil- and Water-Soluble Vitamins with Minerals Capsules. The label also states the quantity of each vitamin and mineral per dosage unit and where necessary the chemical form in which a vitamin is present and also states the salt form of the mineral used as the source of each element. Where the product contains vitamin E, the label indicates whether it is the
d- or
dl- form. Where more than one
Assay method is given for a particular vitamin or mineral, the labeling states with which
Assay method the product complies only if
Method 1 is not used.
Microbial enumeration 
2021
—
The total aerobic microbial count does not exceed 3000 cfu per g, and the combined molds and yeasts count does not exceed 300 cfu per g. Capsules also meet the requirements of the tests for absence of
Salmonella species,
Escherichia coli, and
Staphylococcus aureus.
NOTE—
In the following assays, where more than one
Assay method is given for an individual ingredient, compliance may be determined by following any one of the specified methods, the method used being stated in the labeling only if
Method 1 is not used.
Assay for vitamin A, Method 1—
Proceed as directed in the
Assay for vitamin A,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Transfer the contents of not fewer than 20 Capsules to a suitable container, mix, and weigh. Transfer an accurately weighed portion of the mixture, equivalent to 5 Capsules, to a container having a polytef-lined screw cap.
[NOTE—For hard gelatin Capsules, remove, as completely as possible, the contents of not fewer than 20 Capsules by cutting open the Capsule shells, using a sharp blade if necessary, transferring the shells and their contents to a suitable container, and triturating to a homogeneous mass. Transfer an accurately weighed portion of the mass, equivalent to 5 Capsules, to a container having a polytef-lined screw cap.
] Add 10 mL of dimethyl sulfoxide and 15 mL of
n-hexane, and shake for 45 minutes on a wrist-action shaker in a water bath maintained at 60
.
[NOTE—Set up the wrist-action shaker to ensure that the contents of the container are mixed vigorously and thoroughly.
] Centrifuge at 3000 rpm for 10 minutes, and transfer the hexane layer by means of a pipet to a 100-mL volumetric flask. Add 15 mL of
n-hexane to the dimethyl sulfoxide layer, shake thoroughly for 5 minutes, and transfer the hexane layer by means of a pipet to the 100-mL volumetric flask. Repeat this extraction with three additional 15-mL portions of
n-hexane. Dilute the extracts in the volumetric flask with
n-hexane to volume, and mix. Quantitatively dilute a 10-mL volume of this solution with
n-hexane to obtain a solution having a final concentration of about 15 µg of retinol per mL. Retain the remaining solution for use in the assays for vitamin D, vitamin E, and phytonadione.
Assay for vitamin A, Method 2—
Proceed as directed in the
Assay for vitamin A,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
[NOTE—This preparation is suitable for the determination of vitamin A, vitamin D, and vitamin E, when present in the formulation.
] Accurately weigh not fewer than 20 Capsules in a tared weighing bottle. Using a sharp blade if necessary, carefully open the Capsules, without loss of shell material, and transfer the contents to a 100-mL beaker. Remove any contents adhering to the empty shells by washing with several portions of ether. Discard the washings, and dry the Capsule shells with the aid of a current of dry air. Weigh the empty Capsule shells in the tared weighing bottle, and calculate the net weight of the Capsule contents. Transfer an accurately weighed portion of the Capsule contents, equivalent to about 30 µg of cholecalciferol or ergocalciferol (vitamin D), to a container having a polytef-lined screw cap. If vitamin D is not present in the formulation, use a portion equivalent to about 90 mg of vitamin E. If vitamin E is not present in the formulation, use a portion equivalent to about 2.5 mg of vitamin A. Proceed as directed for
Assay preparation in the
Assay for vitamin A,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add about 0.5 g of sodium bicarbonate.”
Assay for vitamin A, Method 3—
Proceed as directed in the
Assay for vitamin A,
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Accurately weigh not fewer than 20 Capsules in a tared weighing bottle. Using a sharp blade if necessary, carefully open the Capsules, without loss of shell material, and transfer the contents to a 100-mL beaker. Remove any contents adhering to the empty shells by washing with several portions of ether. Discard the washings, and dry the Capsule shells with the aid of a current of dry air. Weigh the empty Capsule shells in the tared weighing bottle, and calculate the net weight of the Capsule contents. Transfer an accurately weighed portion of the Capsule contents, equivalent to about 1.5 mg of retinyl acetate, to a stoppered 125-mL flask, and proceed as directed for
Assay preparation in the
Assay for vitamin A,
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 5 mL of water.”
Assay for cholecalciferol or ergocalciferol (vitamin D), Method 1—
Proceed as directed in the
Assay for cholecalciferol or ergocalciferol (
vitamin D),
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Transfer an accurately measured volume of the solution retained as specified in the directions for Assay preparation in the Assay for vitamin A, Method 1 to a suitable container, and evaporate, if necessary, in vacuum at room temperature to obtain a solution having a concentration of about 2 µg of cholecalciferol or ergocalciferol per mL.
Assay for cholecalciferol or ergocalciferol (vitamin D), Method 2—
Proceed as directed in the
Assay for cholecalciferol or ergocalciferol (
vitamin D),
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for vitamin A, Method 2.
Assay for cholecalciferol or ergocalciferol (vitamin D), Method 3—
Proceed as directed in the
Assay for cholecalciferol or ergocalciferol (
vitamin D),
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for vitamin A, Method 3, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 10 µg of ergocalciferol or cholecalciferol, to a stoppered 125-mL flask, and proceed as directed for Standard preparation, beginning with “Add 15.0 mL of water and 15.0 mL of Potassium hydroxide solution.”
Assay for vitamin E, Method 1—
Proceed as directed in the
Assay for vitamin E,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Transfer not less than 20 mL, accurately measured, of the solution retained as specified in the directions for Assay preparation in the Assay for vitamin A, Method 1 to a suitable container, and evaporate if necessary, in vacuum at room temperature to dryness. Transfer the contents of the flask to a suitable volumetric flask with the aid of methanol, and dilute with methanol to volume to obtain a solution having a concentration of about 2 mg of alpha tocopherol, alpha tocopheryl acetate, or alpha tocopheryl acid succinate per mL.
Assay for vitamin E, Method 2—
Proceed as directed in the
Assay for vitamin E,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
3 N Methanolic sulfuric acid solution,
Sodium ascorbate-pyrogallol solution,
Lecithin solution, and
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for vitamin A, Method 2, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 55 mg of vitamin E, to a container having a polytef-lined screw cap. Add about 0.5 g of sodium bicarbonate, 1.5 mL of Lecithin solution, and 12.5 mL of 2,2,4-trimethylpentane, and disperse on a vortex mixer. Add 6 mL of Sodium ascorbate-pyrogallol solution, shake slowly, and allow the solution to degas. Continue shaking until the evolution of gas has ceased, and then shake for an additional 12 minutes. Add 6 mL of dimethyl sulfoxide, mix on a vortex mixer to form a suspension, and shake for 12 minutes. Add 6 mL of 3 N Methanolic sulfuric acid solution, mix on a vortex mixer to form a suspension, and shake for 12 minutes. Add 12.5 mL of 2,2,4-trimethylpentane, mix on a vortex mixer to form a suspension, and shake for 10 minutes. Centrifuge for about 10 minutes to break up the emulsion and to clarify the supernatant layer. Transfer an accurately measured volume of the supernatant 2,2,4-trimethylpentane layer to a suitable volumetric flask, the volume of the specimen withdrawn from the 2,2,4-trimethylpentane layer and the size of the volumetric flask being such that the final concentration of the Assay preparation is equivalent to that of the Standard preparation. Evaporate nearly to dryness, add several mL of methanol, and evaporate the remaining 2,2,4-trimethylpentane. Dilute with methanol to volume, and mix.
Assay for vitamin E, Method 3—
Proceed as directed in the
Assay for vitamin E,
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for vitamin A, Method 3, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 8.0 mg of alpha tocopherol, to a glass-stoppered conical flask, and proceed as directed for Assay preparation in the Assay for vitamin E, Method 3 under Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 25.0 mL of water.”
Assay for phytonadione—
Proceed as directed in the
Assay for phytonadione under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Transfer not less than 20 mL, accurately measured, of the solution retained as specified in the directions for Assay preparation in the Assay for vitamin A, Method 1 to a suitable container, and evaporate, if necessary, in vacuum at room temperature to dryness. Transfer the contents of the flask to a suitable volumetric flask with the aid of methanol, and dilute with methanol to volume to obtain a solution having a concentration of about 20 µg of phytonadione per mL.
Assay for beta carotene—
Proceed as directed in the
Assay for beta carotene under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use one of the following
Assay preparations.
Assay preparation 1 (for preparations containing beta carotene in oil solutions)—
Proceed as directed in the Assay for vitamin A, Method 1, except to use cyclohexane instead of n-hexane as the extraction solvent and to dilute the filtered extracts quantitatively, and stepwise if necessary, with cyclohexane to obtain a solution having a concentration of about 2 µg of beta carotene per mL.
Assay preparation 2 (for preparations containing beta carotene in dry powder)—
Remove the contents of not fewer than 20 Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the Capsule contents, equivalent to about 2 mg of beta carotene, to a 500-mL saponification flask, and proceed as directed for
Assay preparation in the
Assay for beta carotene under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 100 mL of alcohol.”
Assay for ascorbic acid, Method 1—
Accurately weigh not fewer than 20 Capsules in a tared weighing bottle. Using a sharp blade if necessary, carefully cut open the Capsules, without the loss of shell material, and transfer the contents to a 100-mL beaker. Remove any contents adhering to the empty shells by washing if necessary with several portions of ether. Discard the washings, and dry the Capsule shells with the aid of a current of dry air until the odor of ether is no longer perceptible. Weigh the empty Capsule shells in the tared weighing bottle, and calculate the average net weight per Capsule. Transfer an accurately weighed portion of the Capsule contents, equivalent to about 100 mg of ascorbic acid, to a 200-mL volumetric flask, and proceed as directed in the
Assay for ascorbic acid,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “add about 75 mL of metaphosphoric-acetic acids TS” and calculating the content of ascorbic acid in each Capsule.
Assay for calcium ascorbate, Method 1—
Proceed as directed in the Assay for ascorbic acid, Method 1.
Assay for sodium ascorbate, Method 1—
Proceed as directed in the Assay for ascorbic acid, Method 1.
Assay for biotin, Method 1—
Proceed as directed in the
Assay for biotin,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the
Assay for ascorbic acid,
Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 1 mg of biotin, to a 200-mL volumetric flask. Add 3 mL of dimethyl sulfoxide, and swirl to wet the contents. Place the flask in a water bath at 60
to 70
for 5 minutes. Sonicate for 5 minutes, dilute with water to volume, mix, and filter.
Assay for biotin, Method 2—
Proceed as directed in the
Assay for biotin,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the
Assay for ascorbic acid,
Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 100 µg of biotin, to a 200-mL volumetric flask, add 3 mL of 50 percent alcohol, and swirl to wet the contents. Heat the flask in a water bath at 60
to 70
for 5 minutes. Sonicate for 5 minutes, dilute with diluted alcohol to volume, mix, and filter. Dilute an accurately measured volume of the filtrate quantitatively, and stepwise if necessary, with water to obtain a solution having a concentration of about 0.1 ng per mL.
Assay for cyanocobalamin, Method 1—
Proceed as directed in the
Assay for cyanocobalamin,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the Assay for ascorbic acid, Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 100 µg of cyanocobalamin, to a 250-mL flask. Quantitatively add 100.0 mL of water, and carefully extract for 2 minutes. Filter about 10 mL of the extract, and use the clear filtrate.
Assay for cyanocobalamin, Method 2—
Proceed as directed in the
Assay for cyanocobalamin,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the
Assay for ascorbic acid,
Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 1.0 µg of cyanocobalamin, to an appropriate vessel containing, for each g of Capsule contents taken, 25 mL of an aqueous extracting solution prepared just prior to use to contain, in each 100 mL, 1.29 g of dibasic sodium phosphate, 1.1 g of anhydrous citric acid, and 1.0 g of sodium metabisulfite. Autoclave the mixture at 121
for 10 minutes. Allow any undissolved particles of the extract to settle, and filter or centrifuge, if necessary. Dilute an aliquot of the clear solution with water to obtain a final solution containing vitamin B
12 activity approximately equivalent to that of the
Standard preparation.
Assay for folic acid, Method 1—
Proceed as directed in the
Assay for folic acid,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the Assay for ascorbic acid, Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 0.4 mg of folic acid, to a 50-mL centrifuge tube. Add 25.0 mL of Internal standard preparation, insert a stopper, shake by mechanical means for 10 minutes, and centrifuge. Filter a portion of the clear supernatant, and use the filtrate.
Assay for folic acid, Method 2—
Proceed as directed in the
Assay for folic acid,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for
Assay preparation in the
Assay for vitamin A,
Method 3, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 0.3 mg of folic acid, to a stoppered 125-mL flask. Add 10.0 mL of methanol and 35.0 mL of
Reagent, insert the stopper, shake for 15 minutes in a water bath maintained at 60
, and cool. Filter, discarding the first few mL of the filtrate.
Assay for calcium pantothenate, Method 1—
Proceed as directed in the
Assay for calcium pantothenate,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the Assay for ascorbic acid, Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 15 mg of calcium pantothenate, to a centrifuge tube. Transfer 25.0 mL of the Internal standard preparation to the centrifuge tube, and shake vigorously for 10 minutes. Centrifuge, filter, and use the clear filtrate.
Assay for calcium pantothenate, Method 2—
Proceed as directed in the
Assay for calcium pantothenate,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the Assay for ascorbic acid, Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 50 mg of calcium pantothenate, to a 1000-mL volumetric flask containing 500 mL of water. Add 10 mL of 0.2 N acetic acid and 100 mL of sodium acetate solution (1 in 60), dilute with water to volume, and filter. Dilute an accurately measured volume of this solution quantitatively, and stepwise if necessary, to obtain a solution having approximately the same concentration as that of the Standard preparation.
Assay for calcium pantothenate, Method 3—
Proceed as directed in the
Assay for calcium pantothenate,
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for folic acid, Method 2, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 10 mg of calcium pantothenate, to a 250-mL volumetric flask, add 10 mL of methanol, and swirl the flask to disperse the Capsules contents. Dilute with water to volume, mix, and filter.
Assay for niacin or niacinamide, pyridoxine hydrochloride, riboflavin, and thiamine, Method 1—
Proceed as directed in the
Assay for niacin or niacinamide,
pyridoxine hydrochloride,
riboflavin,
and thiamine,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed in the
Assay for ascorbic acid,
Method 1, through “calculate the average net weight per Capsule.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 10 mg of niacinamide and 2.5 mg each of pyridoxine hydrochloride, riboflavin, and thiamine hydrochloride, to a 50-mL centrifuge tube. Proceed as directed for
Assay preparation in the
Assay for niacin or niacinamide,
pyridoxine hydrochloride,
riboflavin,
and thiamine,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 25.0 mL of
Diluting solution”.
Assay for niacin, Method 2—
Proceed as directed in the
Assay for niacin,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
[NOTE—This preparation is suitable for the determination of niacin or niacinamide, pyridoxine hydrochloride, and riboflavin, when present in the formulation.
] Accurately weigh not fewer than 20 Capsules in a tared weighing bottle. Using a sharp blade if necessary, carefully open the Capsules, without loss of shell material, and transfer the contents to a beaker. Remove any contents adhering to the shells by washing with several portions of ether. Discard the washings, and dry the Capsule shells with the aid of a current of dry air. Weigh the empty Capsule shells in the tared weighing bottle, and calculate the net weight of the Capsule contents. Transfer an accurately weighed portion of the Capsule contents, equivalent to about 2 mg of riboflavin, to a 250-mL volumetric flask. If riboflavin is not present in the formulation, use a portion equivalent to about 2 mg of pyridoxine. If pyridoxine is not present in the formulation, use a portion equivalent to about 20 mg of niacin or niacinamide. Add 100.0 mL of
Extraction solvent, and mix for 20 minutes, using a wrist-action shaker. Immerse the flask in a water bath maintained at 70
to 75
, and heat for 20 minutes. Mix on a vortex mixer for 30 seconds, cool to room temperature, and filter. Use the clear filtrate.
Assay for niacinamide, Method 2—
Proceed as directed in the
Assay for niacinamide,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Prepare as directed for Assay preparation in the Assay for niacin, Method 2.
Assay for pyridoxine hydrochloride, Method 2—
Proceed as directed in the
Assay for pyridoxine hydrochloride,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Prepare as directed for the Assay preparation in the Assay for niacin, Method 2.
Assay for riboflavin, Method 2—
Proceed as directed in the
Assay for riboflavin,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Prepare as directed for Assay preparation in the Assay for niacin, Method 2.
Assay for thiamine, Method 2—
Proceed as directed in the
Assay for thiamine,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for vitamin A, Method 3, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the contents, equivalent to about 2 mg of thiamine, to a 250-mL volumetric flask. Add 100.0 mL of 0.2 N hydrochloric acid, shake for 15 minutes with a wrist-action shaker, and heat to boiling for 30 minutes. Cool to room temperature, and filter. Use the clear filtrate.
Assay for niacin or niacinamide, pyridoxine hydrochloride, riboflavin, and thiamine, Method 3—
Proceed as directed in the
Assay for niacin or niacinamide,
pyridoxine hydrochloride,
riboflavin,
and thiamine,
Method 3 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Proceed as directed for
Assay preparation in the
Assay for vitamin A,
Method 3, through “calculate the net weight of the Capsule contents.” Transfer an accurately weighed portion of the Capsule contents, equivalent to about 7.5 mg of niacin or niacinamide, 1.2 mg of pyridoxine hydrochloride, 0.4 mg of riboflavin, and 1.2 mg of thiamine hydrochloride, to a stoppered 125-mL flask. Add 10.0 mL of a mixture of methanol and glacial acetic acid (9:1) and 30.0 mL of a mixture of methanol and ethylene glycol (1:1). Insert the stopper, shake for 15 minutes in a water bath maintained at 60
, and cool. Filter, discarding the first few mL of the filtrate.
NOTE—Commercially available atomic absorption standard solutions for the minerals, where applicable, may be used where preparation of a standard stock solution is described in the following Assays. Use deionized water where water is specified. Where atomic absorption spectrophotometry is specified in the Assay, the Standard preparations and the Assay preparation may be diluted quantitatively with the solvent specified, if necessary, to yield solutions of suitable concentrations adaptable to the linear or working range of the instrument.
Assay for calcium—
Proceed as directed in the
Assay for calcium under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Dilute 100 mL of polysorbate 80 with alcohol to 1000 mL.
Assay preparation—
Transfer 5 Capsules to a 100-mL volumetric flask. [NOTE—For hard gelatin Capsules, accurately weigh not fewer than 20 Capsules. Using a sharp blade if necessary, carefully open the Capsules, without loss of shell material, and transfer the contents to a suitable container. Remove any contents adhering to the empty shells by washing with several portions of ether. Discard the washings, and allow the Capsule shells to dry. Weigh the empty Capsule shells, calculate the net weight of the Capsule contents, and transfer an accurately weighed portion of the Capsule contents, equivalent to about 5 Capsules, to a 100-mL volumetric flask.] Add about 15 mL of water, 10 mL of 6 N hydrochloric acid, and about 1 mL of Polysorbate 80 solution to the flask, and heat on a hot plate or steam bath, with intermittent swirling, until the Capsules are completely disintegrated or the contents are dissolved. Boil gently for an additional 15 minutes. Cool, dilute with water to volume, and filter, discarding the first 5 mL of the filtrate. Dilute this solution quantitatively, and stepwise if necessary, with 0.125 N hydrochloric acid to obtain a solution having a known concentration of about 2 µg of calcium per mL, adding 1 mL of Lanthanum chloride solution per 100 mL of the final volume.
Assay for chromium—
Proceed as directed in the
Assay for chromium under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 1 µg of chromium per mL and to omit the use of the Lanthanum chloride solution.
Assay for copper—
Proceed as directed in the
Assay for copper under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 2 µg of copper per mL and to omit the use of the Lanthanum chloride solution.
Assay for fluoride, Method 1—
Proceed as directed in the
Assay for fluoride,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the contents, equivalent to about 200 µg of fluoride, to a 100-mL volumetric flask. Add 10.0 mL of 1 N hydrochloric acid, 25.0 mL of 3 M Sodium acetate solution, and 25.0 mL of Sodium citrate solution, dilute with water to volume, and mix.
Assay for fluoride, Method 2—
Proceed as directed in the
Assay for fluoride,
Method 2, under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Accurately weigh not fewer than 20 Capsules in a tared weighing bottle. Using a sharp blade if necessary, carefully open the Capsules, without loss of shell material, and transfer the contents to a 100-mL container. If necessary, remove any contents adhering to the empty shells by washing with several portions of ether. Discard the washings, and dry the Capsule shells with the aid of a current of dry air. Weigh the empty Capsule shells in the tared weighing bottle, and calculate the net weight of the Capsule contents. Transfer an accurately weighed portion of the Capsule contents, equivalent to about 1 mg of fluoride, to a 100-mL volumetric flask. Proceed as directed for
Assay preparation in the
Assay for fluoride,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “add 15 mL of water”.
Assay for iodide, Method 1—
Bromine water—
To about 20 mL of bromine in a glass-stoppered bottle, add 100 mL of water. Insert the stopper into the bottle, and shake. Allow to stand for 30 minutes, and use the supernatant layer.
Procedure—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the contents, equivalent to about 3 mg of iodine, to a nickel crucible. Proceed as directed for
Procedure in the
Assay for iodide,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 5 g of sodium carbonate.”
Assay for iron—
Proceed as directed in the
Assay for iron under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 5 µg of iron per mL and to omit the use of the Lanthanum chloride solution.
Assay for magnesium—
Proceed as directed in the
Assay for magnesium under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 0.4 µg of magnesium per mL.
Assay for manganese—
Proceed as directed in the
Assay for manganese under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 1 µg of manganese per mL and to omit the use of the Lanthanum chloride solution.
Assay for molybdenum, Method 1—
Proceed as directed in the
Assay for molybdenum,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to take a number of Capsules or a portion of Capsule contents equivalent to about 1000 µg of molybdenum and to make appropriate dilutions to obtain a final concentration of about 10 µg of molybdenum per mL, omitting the addition of the Lanthanum chloride solution.
Assay for molybdenum, Method 2—
Proceed as directed in the
Assay for molybdenum,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Procedure.
Procedure—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the Capsule contents, equivalent to about 40 µg of molybdenum, to a 200-mL beaker, marked
I. Proceed as directed for
Procedure in the
Assay for molybdenum,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “To another 200-mL beaker”, except to read Capsules in place of Tablets.
Assay for phosphorus—
Proceed as directed in the
Assay for phosphorus under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the Capsule contents, equivalent to about 100 mg of phosphorus, to a suitable flask. Proceed as directed for
Assay preparation in the
Assay for phosphorus under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “add 25 mL of nitric acid”.
Assay for potassium—
Proceed as directed in the
Assay for potassium under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 1 µg of potassium per mL and to omit the use of the Lanthanum chloride solution.
Assay for selenium, Method 1—
Proceed as directed in the
Assay for selenium,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the Capsule contents, equivalent to about 1000 µg of selenium, to a suitable flask. Proceed as directed for
Assay preparation in the
Assay for selenium,
Method 1 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “and add about 12 mL of nitric acid.”
Assay for selenium, Method 2—
Proceed as directed in the
Assay for selenium,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Assay preparation.
Assay preparation—
Remove the contents of a counted number of Capsules by cutting open the Capsules, using a sharp blade if necessary. Mix, and determine the weight of the contents. Transfer an accurately weighed quantity of the Capsule contents, equivalent to about 20 µg of selenium, to a suitable flask. Proceed as directed for
Assay preparation in the
Assay for selenium,
Method 2 under
Oil- and Water-Soluble Vitamins with Minerals Tablets, beginning with “Add 10 mL of nitric acid.”
Assay for zinc—
Proceed as directed in the
Assay for zinc under
Oil- and Water-Soluble Vitamins with Minerals Tablets, except to read Capsules in place of Tablets and to use the following
Polysorbate 80 solution and
Assay preparation.
Polysorbate 80 solution—
Prepare as directed in the Assay for calcium.
Assay preparation—
Proceed as directed for Assay preparation in the Assay for calcium, except to prepare the Assay preparation to contain about 2 µg of zinc per mL and to omit the use of the Lanthanum chloride solution.
