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First Published: Third Supplement, FCC 7

Low Glycemic Carbohydrate DESCRIPTION Sucromalt occurs as a clear, colorless to light yellow, slightly cloudy liquid. It is the product of an enzyme-catalyzed reaction of sucrose and maltose, combined at a specific ratio. The reaction is pH- and temperature-controlled and utilizes a food-grade glucosyltransferase enzyme. The resulting syrup may be further treated to deactivate the enzyme, purified, and evaporated under vacuum to obtain an optimal dry solids content. Sucromalt is composed of 35%45% fructose, 7%15% leucrose, less than 5% other mono- and di-saccharides, and 40%60% higher glucooligosaccharides of 12+ DP. Function: Source of slowly digestible nutritive carbohydrate Packaging and Storage: Store in well-closed containers. IDENTIFICATION
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H NMR SPECTROSCOPY, Nuclear Magnetic Resonance Spectroscopy, Appendix IIC Solvent: Use deuterium oxide (D2O, 99.999% atom D) that contains 0.01% (v/v) dimethylsulfoxide (DMSO) as an internal intensity standard and 0.01% (w/v) sodium 3,3,4,4,5,5-hexadeutero-2,2-dimethyl-2-silapentane-5-sulfonate (DSS-d6) as an internal chemical shift standard. Standard solution: Prepare a solution in Solvent containing 5 mg/mL of USP Sucromalt RS. Vortex the mixture for 10 min at room temperature, then centrifuge at 7200 g for 10 min. Transfer 600-L aliquots of the supernatant to 5-mm NMR tubes, and sonicate for 10 min to eliminate air bubbles. Sample solution: Prepare a solution in Solvent containing 5 mg/mL of Sucromalt. Vortex the mixture for 10 min at room temperature, then centrifuge at 7200 g for 10 min. Transfer 600-L aliquots of the supernatant to 5-mm NMR tubes, and sonicate for 10 min to eliminate air bubbles. Analysis: Collect H NMR spectra of the Standard solution and Sample solution at 25 . Compare the data collected between 4.80 ppm and 5.50 ppm within the anomeric region of the spectrum. For the spectrum obtained from the Sample solution, identify the signals due to -(1,6) and -(1,3) glycosidic linkages by comparison to the Reference
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Spectrum provided with the USP Sucromalt RS. Calculate the ratio of the intensities of the H signals due to the and -(1,3) glycosidic linkages in the spectrum obtained for the Sample solution.

-(1,6)

Acceptance criteria: The spectrum obtained for the Sample solution exhibits a chemical shift pattern with signal locations and intensities that match those obtained from the Standard solution within the defined chemical shift range of 4.805.50 ppm. The ASSAY PROCEDURE Mobile phase: Degassed, purified water passed through a 0.22-m filter before use. The conductivity should be NMT 1 megaohm. [NOTE Maintain the water at 85 during operation of the chromatograph.] Standard solution: Prepare a solution containing a total of about 10% solids, using sugars of known purity (e.g., USP Fructose RS, USP Dextrose RS, USP Maltose Monohydrate RS, or NIST Standard Reference Material; leucrose; or equivalent) that approximates, on the dry basis, the composition of the sample to be analyzed. Dissolve each standard sugar in 20 mL of purified water contained in a 50-mL beaker. Heat on a steam bath until all sugars are dissolved, then cool, and transfer to a 100-mL volumetric flask. Dilute with water to volume, and mix. [NOTE Freeze the solution if it is to be reused.] Sample solution: Dilute to approximately 7%12% solids and filter through a syringe filter system. Chromatographic system, Appendix IIA
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-(1,6)/ -(1,3) signal ratio for the Sample solution is within the range 1.41.9.

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[NOTE Use a suitable high-performance liquid chromatography system. ] Mode: High-performance liquid chromatography Detector: Differential refractometer Column: 22- to 31-cm stainless steel column, or equivalent with a stationary phase of prepacked macroreticular polystyrene sulfonated divinylbenzene cation-exchange resin (2%8% cross-linked, 8- to 25-m particle size), preferably in the calcium or silver form. Examples of acceptable resins are Bio-Rad Aminex HPX-87C, or equivalent, for separating DP1DP4 saccharides, and Aminex HPX-42C and HPX-42A, or equivalent, for separating DP1DP7 saccharides. [NOTE Condition the column before use by pumping solvent at 0.1 mL/min through the column while bringing it to operating temperature. Increase the flow rate to 0.5 mL/min, and allow to equilibrate for 45 min prior to use.] Temperature Column: 85 Detector: 45 Flow rate: 0.51.0 mL/min Injection volume: 10 L Standardization: If a corn syrup or maltodextrin is used to supply a DP4+ fraction, take care to include all saccharides in the standard composition calculation. Calculate the dry-basis concentration, as a percentage, of each individual component in the Standard solution: Result = (W C/SW I) 100

WC = weight of the sugar of interest SWI = sum of the weights of all sugar components
Standardize by injecting 1020 L (about 1.02.0 mg of solids) of the Standard solution into the chromatograph. Integrate the peaks and normalize. Sum the individual DP4+ responses from the normalized printout to obtain the total DP4+ normalized response. Calculate the response factors: RI = (known concentration, dry basis %)/(measured concentration, normalized %)

RI = response factor for component i

Compute the response factor for each component relative to glucose (R'I): R'I = RI/RG

R'I = response factor relative to glucose for component i RI = response factor for component i RG = response factor for glucose
The R'I for DP4+ should be programmed as a default value (if automated equipment is used) and used to compute the concentration of higher saccharides. Analysis: Inject a volume of the Sample solution into the chromatograph and record the resulting chromatogram. Calculate the concentration of each component: CI = (AI RI 100)/(SANRN)

CI AI RI

= concentration of component i = peak area recorded for component i = response factor for component i = sum of the product of the areas (A) and response factors (R) for all components SANRN detected

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Acceptance criteria Fructose: 35%45%, calculated on the dry basis Leucrose: 7%15%, calculated on the dry basis Higher saccharides and polymer: NLT 40%, calculated on the dry basis DP2: NMT 5%, calculated on the dry basis IMPURITIES Inorganic Impurities LEAD , Lead Limit Test, Atomic Absorption Spectrophotometric Graphite Furnace Method, Method I, Appendix IIIB Sample: 5 g Acceptance criteria: NMT 0.1 mg/kg SULFUR DIOXIDE, Sulfur Dioxide Determination, Appendix X Sample: 50 g [NOTE Alternately, the following method may be used.] Solution A: Dissolve 40 g of potassium iodide in 200 mL of water in a 1-L volumetric flask. Allow the solution to come to room temperature, add 12.7 g of crystalline iodine, and stir until the iodine is completely dissolved. Add 3 drops of concentrated hydrochloric acid, and dilute with water to volume. Mix the solution thoroughly, and store in an actinic glass bottle. Solution B: Dilute 2 mL of Solution A with water to 100 mL (0.002 N iodine). Indicator solution: Prepare a slurry of 10 g of soluble starch (Lintner) in 50 mL of cold water. Quantitatively transfer the slurry to 1 L of boiling water and stir, with boiling, until dissolved. Allow the solution to cool to room temperature before use. Sample: 50 g Analysis: Transfer the Sample to a 250-mL beaker, add 75 mL of water, and mix well. Transfer the solution to a 250-mL Erlenmeyer flask, and cool to 25 . Add 10 mL of cold 1.3 N potassium hydroxide to the flask, and stir, then immediately add 10 mL of cold 1.5 N sulfuric acid, and stir. Add a few drops of the Indicator solution, and titrate immediately with Solution B until the blue color remains for 30 s. Perform a blank titration (see General Provisions). Calculate the sulfur dioxide content, in ppm, of the sample: Result = (VU VB) NI F1 (1/W U) F2

VU = volume of titrant required for the sample titration (mL) VB = volume of titrant required for the blank titration (mL) NI = normality of the iodine solution, Solution B F1 = milliequivalent weight of sulfur dioxide (64.071/2 1000), 0.032 WU = weight of the Sample (g) F2 = factor converting g to mg and g to kg, 1,000,000
Acceptance criteria: NMT 5 ppm SPECIFIC TESTS M OISTURE Filter aid: Use a celite diatomite filter aid such as Hyflo Super-Cel, or equivalent. [NOTE Do not substitute an acidwashed diatomaceous earth filter aid.] Wash a large quantity of the filter aid by percolation on a Buchner funnel with water acidified with hydrochloric acid (1 mL of concentrated hydrochloric acid per L of water). Continue washing until the effluent is acid to litmus, then wash the filter aid with water until the effluent is pH 4 or above. Air dry the washed filter aid for storage. Before use, dry a quantity of the prepared filter aid overnight in an oven maintained at 105 , then store in a closed container. Sample: Amount of material equivalent to 47 g of dry substance Apparatus: Use a vacuum oven with uniform heat distribution and that is capable of maintaining the vacuum for several hours when the pump is shut off. The air inlet of the oven should be attached to a drying tower filled with a calcium
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sulfate desiccant with added moisture indicator. The tower should be connected in series to a gas scrubber containing concentrated sulfuric acid. Stirrers: Use 100-mm 13-mm borosilicate glass test tubes equipped with extensions. The extensions should be made from 8-mm 180-mm stainless steel rods. Near one end of each rod, place two rubber rings (use appropriately-sized rubber o-rings or rings cut from rubber tubing) spaced such that when the rod is inserted into the test tube, it fits snugly at the top and bottom of the tube. Analysis: Transfer about 30 g of Filter aid to a 3-in diameter aluminum drying dish. Use dishes that are about 3.5-in high that are fitted with aluminum lids. Prepare two dishes: one for the sample analysis and one for a blank. Place one of the test tube Stirrers (without the stainless steel rod) in each sample dish. Dry the dishes uncovered in the vacuum oven described under Apparatus at 100 and NMT 25 torr while bleeding a small current of air through the oven and its drying tower. Continue drying for 5 h, then shut off the vacuum, and allow the oven to slowly fill with air drawn through the drying tower. Open the oven, quickly cover the dishes with their lids, then place the dishes in a desiccator, and allow them to cool to room temperature before weighing. Once the dishes are completely cooled, remove them from the desiccator, release the closure, and immediately weigh. Record all weights to the nearest mg. Weigh the Sample into a 45-mL weighing bottle equipped with a cap style ground glass stopper. Add 10 mL of warm water, and stir with a glass rod. Pour the diluted material onto the prepared Filter aid in one of the aluminum weighing dishes, using three 5-mL portions of warm water to assist the quantitative transfer. Insert the steel extension rod described in Stirrers into the sample dish, and stir until the mixture is homogenous and evenly dispersed. Remove the rod from the test tube, leaving the stirring tube in the dish. Place dishes for the blank and the sample, uncovered, in the vacuum oven. [NOTE Set the oven at 70 for samples with a DE of over 58 (and for all samples containing fructose) and at 100 for samples with a DE of 58 and below.] Allow the materials to dry for 5 h in the vacuum oven, then remove the dishes from the oven. Re-insert the stainless steel rods into the test tube Stirrers, and stir the material in the dish until a fine powder free of lumps is obtained. Return the dishes to the oven, and continue heating for an additional 1516 h. Once the heating period is over, shut off the vacuum line and allow the oven to slowly fill with air drawn through the drying tower. Open the oven, quickly cover the dishes with their lids, then place the dishes in a desiccator, and allow them to cool to room temperature before weighing. Once the dishes are completely cooled, remove them from the desiccator, release the closure, and immediately weigh. Record all weights to the nearest mg, and calculate the percent moisture in the Sample. Acceptance criteria: NMT 30.0% PH, pH Determination, Appendix IIB Sample solution: 10% (w/w) Analysis: Proceed as directed using pH 4.00 and 7.00 standard buffer solutions to calibrate the pH meter. Acceptance criteria: 3.56.0
3S (FCC 7) 1 Aldrich Chemical Company. 2 Such as the one described in Standard Analytical Methods of the Corn Refiners Association, available from the Corn Refiners Association, Washington, DC. 3 Available from Johns-Manville Products Corp., Lompoc, CA. 4 Drierite, or equivalent.

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Expert Committee (FI2010) Monographs - Food Ingredients

FCC Seventh Edition Supplement 3 Page 1714

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