Maltitol syrup

Prepared at the 49th JECFA (1997)
superseding specifications prepared at the 46th JECFA (1996),
published in FNP 5 2 Addendum 4 (1996)

SYNONYMS

Hydrogenated high maltose-content glucose syrup, hydrogenated glucose syrup, dried maltitol syrup, maltitol syrup powder INS No. 965

DEFINITION

A mixture consisting of mainly maltitol with sorbitol and hydrogenated oligo-and polysaccharides. It is manufactured by the catalytic hydrogenation of high maltose-content glucose syrup. The article of commerce is typically supplied as a syrup. It may also be dried and supplied as a solid product

Assay

Not less than 99.0% of total hydrogenated saccharides on the anhydrous basis and not less than 50.0% of maltitol on the anhydrous basis

DESCRIPTION

Colourless and odourless, clear viscous liquids or white crystalline masses

FUNCTIONAL USES

Sweetener, humectant, texturizer, stabilizer, bulking agent

CHARACTERISTICS

IDENTIFICATION TESTS

Solubility

Very soluble in water, slightly soluble in ethanol

Thin layer chromatography

Passes test See description under TESTS

PURITY TESTS

Water

Not more than 31% (Karl Fischer)

Sulfated ash

Not more than 0.1 %
Test 3 g of sample as directed under the test for Ash (Sulfated ash) Method I

Chloride

Not more than 50 mg/kg
Test 10 g of the sample by the Limit Test using 1.5 ml of 0.01 N hydrochloric acid in the standard

Sulfate

Not more than 100 mg/kg Test 10 g of the sample by the Limit Test using 2.0 ml of 0.01 N sulfuric acid in the standard

Nickel

Not more than 2 mg/kg
See description under TESTS

Lead

Not more than 1 mg/kg
Prepare a sample solution as directed for organic compounds in the Limit Test and determine the lead content by atomic absorption spectrometry

Reducing sugars

Not more than 0.3%
Proceed as described in the method for Reducing Substances (as glucose), Method II. The weight of cuprous oxide shall not exceed 50 mg

TESTS

IDENTIFICATION TEST

Thin layer chromatography

Examine by thin layer chromatography using silica gel as the coating substance
Standard solution:
Dissolve 50 mg of reference standard maltitol (available from US Pharmacopeial Convention, Inc., 12601 Twinbrook Parkway, Rockville, MD 20852, USA) in 20 ml water
Test solution:
Dissolve 50 mg of sample in 20 ml of water
4-Aminobenzoic acid reagent:
Prepare a solution by dissolving 1 g of 4-aminobenzoic acid in a solvent mixture composed of 18 ml acetic acid, 20 ml water and 1 ml phosphoric acid. Prepare this reagent immediately before use.
Sodium periodate reagent:
A solution of 0.2% w/v sodium periodate in water
Procedure:
Apply 2 m l of each of the standard and test solution to the bottom of the TLC plate. Develop the chromatogram over a path of 17 cm using as the mobile phase a mixture of 70 volumes of propanol, 20 volumes of ethyl acetate and 10 volumes of water. Allow the plate to dry in air and spray with a mixture of 2 volumes of 4-aminobenzoic acid reagent with 3 volumes of acetone. Heat at 100° for 15 min. Spray with the sodium periodate reagent. Heat at 100° for 15 min. The principal spot in the chromatogram obtained from the test solution corresponds in position, colour and size to the principal spot obtained from the standard solution.

PURITY TESTS

Nickel

Test solution:
Dissolve 20.0 g of the sample in a mixture of equal volumes of dilute acetic acid TS and water and dilute to 100 ml with the same mixture of solvents. Add 2.0 ml of a 1% w/v solution of ammonium pyrrolidinedithiocarbamate and 10 ml of methyl isobutyl ketone. Mix and allow the layers to separate and use the methyl isobutyl ketone layer for analysis.
Standard solutions:
Prepare three standard solutions in the same manner as the test solution but adding 0.5 ml, 1.0 ml, and 1.5 ml, respectively, of a standard nickel solution containing 10 mg/l Ni, in addition to the 20.0 g of the sample.
Procedure:
Set the instrument to zero using methyl isobutyl ketone prepared as described for the preparation of the test solution but omitting the substance to be examined. Use a nickel hollow-cathode lamp as source of radiation and an air-acetylene flame. The analysis wavelength for all solutions is 232.0 nm.

METHOD OF ASSAY

Total hydrogenated saccharides (%):

Maltitol is determined by High Performance Liquid Chromatography (HPLC) using the following conditions:
Apparatus:
- Detection: Differential refractometer maintained at constant temperature
- Integrator recorder -Liquid chromatograph (HPLC)
- Column: AMINEX HPX 87 C (resin in calcium form), length 30 cm, internal diameter 9 mm
- Eluent: Double distilled degassed water (filtered through Millipore membrane filter 0.45 m m)
Chromatographic conditions:
Column temperature: 85 ± 0.5°
Eluent flow rate: 0.5 ml/min
Standard preparation:
Dissolve an accurately weighed quantity of standard reference maltitol (available from US Pharmacopeial Convention Inc., 12601 Twinbrook Parkway, Rockville, MD 20852, USA) in water to obtain a solution having known concentration of about 10.0 mg of maltitol per ml.
Sample preparation:
Transfer about 1 g of the sample accurately weighed to a 50-ml volumetric flask, dilute with water to volume and mix.
Procedure:
Separately inject equal volumes (about 20 m l) of the sample preparation and the standard preparation into the chromatograph. Record the chromatograms and measure the responses of each maltitol peak. Calculate the quantity, in mg, of maltitol in the syrup by the following formula:

in which C is the concentration, in mg per ml, of maltitol in the standard preparation; R_U is the peak response of maltitol from the sample preparation and R_S is the peak response of the standard preparation.

SYNONYMS	Hydrogenated high maltose-content glucose syrup, hydrogenated glucose syrup, dried maltitol syrup, maltitol syrup powder INS No. 965
DEFINITION	A mixture consisting of mainly maltitol with sorbitol and hydrogenated oligo-and polysaccharides. It is manufactured by the catalytic hydrogenation of high maltose-content glucose syrup. The article of commerce is typically supplied as a syrup. It may also be dried and supplied as a solid product
Assay	Not less than 99.0% of total hydrogenated saccharides on the anhydrous basis and not less than 50.0% of maltitol on the anhydrous basis
DESCRIPTION	Colourless and odourless, clear viscous liquids or white crystalline masses
FUNCTIONAL USES	Sweetener, humectant, texturizer, stabilizer, bulking agent
CHARACTERISTICS
IDENTIFICATION TESTS
Solubility	Very soluble in water, slightly soluble in ethanol
Thin layer chromatography
	Passes test See description under TESTS
PURITY TESTS
Water	Not more than 31% (Karl Fischer)
Sulfated ash	Not more than 0.1 % Test 3 g of sample as directed under the test for Ash (Sulfated ash) Method I
Chloride	Not more than 50 mg/kg Test 10 g of the sample by the Limit Test using 1.5 ml of 0.01 N hydrochloric acid in the standard
Sulfate	Not more than 100 mg/kg Test 10 g of the sample by the Limit Test using 2.0 ml of 0.01 N sulfuric acid in the standard
Nickel	Not more than 2 mg/kg See description under TESTS
Lead	Not more than 1 mg/kg Prepare a sample solution as directed for organic compounds in the Limit Test and determine the lead content by atomic absorption spectrometry
Reducing sugars	Not more than 0.3% Proceed as described in the method for Reducing Substances (as glucose), Method II. The weight of cuprous oxide shall not exceed 50 mg
TESTS
IDENTIFICATION TEST
Thin layer chromatography
	Examine by thin layer chromatography using silica gel as the coating substance Standard solution: Dissolve 50 mg of reference standard maltitol (available from US Pharmacopeial Convention, Inc., 12601 Twinbrook Parkway, Rockville, MD 20852, USA) in 20 ml water Test solution: Dissolve 50 mg of sample in 20 ml of water 4-Aminobenzoic acid reagent: Prepare a solution by dissolving 1 g of 4-aminobenzoic acid in a solvent mixture composed of 18 ml acetic acid, 20 ml water and 1 ml phosphoric acid. Prepare this reagent immediately before use. Sodium periodate reagent: A solution of 0.2% w/v sodium periodate in water Procedure: Apply 2 m l of each of the standard and test solution to the bottom of the TLC plate. Develop the chromatogram over a path of 17 cm using as the mobile phase a mixture of 70 volumes of propanol, 20 volumes of ethyl acetate and 10 volumes of water. Allow the plate to dry in air and spray with a mixture of 2 volumes of 4-aminobenzoic acid reagent with 3 volumes of acetone. Heat at 100° for 15 min. Spray with the sodium periodate reagent. Heat at 100° for 15 min. The principal spot in the chromatogram obtained from the test solution corresponds in position, colour and size to the principal spot obtained from the standard solution.
PURITY TESTS
Nickel	Test solution: Dissolve 20.0 g of the sample in a mixture of equal volumes of dilute acetic acid TS and water and dilute to 100 ml with the same mixture of solvents. Add 2.0 ml of a 1% w/v solution of ammonium pyrrolidinedithiocarbamate and 10 ml of methyl isobutyl ketone. Mix and allow the layers to separate and use the methyl isobutyl ketone layer for analysis. Standard solutions: Prepare three standard solutions in the same manner as the test solution but adding 0.5 ml, 1.0 ml, and 1.5 ml, respectively, of a standard nickel solution containing 10 mg/l Ni, in addition to the 20.0 g of the sample. Procedure: Set the instrument to zero using methyl isobutyl ketone prepared as described for the preparation of the test solution but omitting the substance to be examined. Use a nickel hollow-cathode lamp as source of radiation and an air-acetylene flame. The analysis wavelength for all solutions is 232.0 nm.
METHOD OF ASSAY	Total hydrogenated saccharides (%): Maltitol is determined by High Performance Liquid Chromatography (HPLC) using the following conditions: Apparatus: - Detection: Differential refractometer maintained at constant temperature - Integrator recorder -Liquid chromatograph (HPLC) - Column: AMINEX HPX 87 C (resin in calcium form), length 30 cm, internal diameter 9 mm - Eluent: Double distilled degassed water (filtered through Millipore membrane filter 0.45 m m) Chromatographic conditions: Column temperature: 85 ± 0.5° Eluent flow rate: 0.5 ml/min Standard preparation: Dissolve an accurately weighed quantity of standard reference maltitol (available from US Pharmacopeial Convention Inc., 12601 Twinbrook Parkway, Rockville, MD 20852, USA) in water to obtain a solution having known concentration of about 10.0 mg of maltitol per ml. Sample preparation: Transfer about 1 g of the sample accurately weighed to a 50-ml volumetric flask, dilute with water to volume and mix. Procedure: Separately inject equal volumes (about 20 m l) of the sample preparation and the standard preparation into the chromatograph. Record the chromatograms and measure the responses of each maltitol peak. Calculate the quantity, in mg, of maltitol in the syrup by the following formula: in which C is the concentration, in mg per ml, of maltitol in the standard preparation; R_U is the peak response of maltitol from the sample preparation and R_S is the peak response of the standard preparation.