Compressible Sugar

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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1 DEFINITION

Compressible Sugar contains NLT 95.0% and NMT 98.0% of sucrose (C₁₂H₂₂O₁₁) on the dried basis. It may contain starch, maltodextrin, or invert sugar and may contain a suitable lubricant.

2 IDENTIFICATION

A. It meets the requirements of the test for Specific Rotation in Specific Tests.

Change to read:

B.SPECTROSCOPIC IDENTIFICATION TESTS (197). Infrared Spectroscopy: 197K (CN 1-Mar-2020)

3 ASSAY

CONTENT OF SUCROSE

Mobile phase: Acetonitrile and water (80:20, v/v)

System suitability solution: Prepare an aqueous solution containing 20 mg/mL of sucrose, 1.0 mg/mL of dextrose (Glucose), 0.6 mg/ml. of fructose, 0.6 mg/mL of maltose, and 0.8 mg/mL of lactose using USP Sucrose RS USP Dextrose RS, USP Fructose RS, USP Maltose

Monohydrate RS, and USP Anhydrous Lactose RS.

Standard solution: Dissolve USP Sucrose RS in water to obtain a solution having a concentration of about 20 mg/mL of sucrose.

Sample solution: 20 mg/mL of Compressible Sugar in water. Pass the solution through a 0.2-um nylon syringe filter.

Chromatographic system

(See Chromatography (621) System Suitability)

Mode: LC

Detector: Refractive index

Column: 4.6-mm x 15-cm; 5-um packing 18

Temperatures

Column: 45°

Detector: 40°

Flow rate: 2.0 mL/min

Injection volume: 15 µL

System suitability

Samples: System suitability solution and Standard solution

[NOTE-For relative retention times, see Table 1.]

Suitability requirements

Resolution: NLT 1.3 between all adjacent peaks, System suitability solution.

Relative standard deviation: NMT 2.0%, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate, on the dried basis, the percentage of sucrose (C12H22O11) in the portion of Compressible Sugar taken:

Result = (r_u/r_s) x (C_s/C_u) × 100

r_u = peak response from the Sample solution

r_s = peak response from the Standard solution

Cs = concentration of USP Sucrose RS in the Standard solution (mg/mL)

C_u = concentration of Compressible Sugar in the Sample solution (mg/mL)

Acceptance criteria: 95.0%-98.0% on the dried basis

4 IMPURITIES

RESIDUE ON IGNITION (281): NMT 0.1%

CHLORIDE AND SULFATE, Chloride(221)

Standard solution: 0.40 ml of 0.020 N hydrochloric acid

Sample solution: Transfer 20 g to a 100-ml volumetric flask, add 80 mL of water, shake to dissolve the sucrose, and then add water to volume. Separate the solubilized sucrose from any insoluble matter by filtration until the filtrate is clear, and use the freshly prepared, clear filtrate.

Acceptance criteria: 0.014%; a 10-ml portion of the Sample solution shows no more chloride than the Standard solution.

CHLORIDE AND SULFATE, Sulfate(221)

Standard solution: 0.50 mL of 0.020 N sulfuric acid.

Sample solution: 25 mL of the Sample solution from the test for Chloride and Sulfate (221), Chloride

Acceptance criteria: 0.010%; the Sample solution shows no more sulfate than the Standard solution.

Change to read:

LIMIT OF CALCIUM (ERR 1-Jun-2018)

Sample solution: 5 ml of the Sample solution from the test for Chloride and Sulfate (221), Chloride

Analysis: To the Sample solution add 1 mL of ammonium oxalate TS.

Acceptance criteria: The solution remains clear for NLT 1 min.

LIMIT OF DEXTROSE (GLUCOSE), FRUCTOSE, MALTOSE, AND LACTOSE

Mobile phase, System suitability solution, Sample solution, and Chromatographic system: Proceed as directed in the test for Content of Sucrose in the Assay.

System suitability

Sample: System suitability solution

[NOTE-The relative retention times for fructose, dextrose (glucose), sucrose, maltose, and lactose are 0.5, 0.6, 1.0, 1.3, and 1.5, respectively.]

Suitability requirements

Resolution: NLT 1.3 between all adjacent peaks

Acceptance criteria: The sum of the peak areas for dextrose, fructose, maltose, and lactose from the Sample solution is less than one third of

the sum of the peak areas for dextrose, fructose, maltose, and lactose from the System suitability solution, corresponding to NMT 5% for the sum of dextrose, fructose, maltose, and lactose.

5 SPECIFIC TESTS

SPECIFIC ROTATION

Sample solution: Transfer 26.0 g of Compressible Sugar, previously dried, to a 100-mL volumetric flask. Add 0.3 mL of a saturated aqueous solution of lead acetate, shake with 90 mL of water, and dilute with water to volume. Distribute evenly on the surface of a sheet of medium-fast filter paper 8 g of chromatographic siliceous earth suitable for column partition chromatography (see Reagents, Indicators, and Solutions-Reagents), and filter the solution, with the aid of vacuum, discarding the first 20 mL of the filtrate.

Instrumental conditions

(See Optical Rotation (781).)

Mode: Specific rotation

Temperature: 20°

Analysis

Uninverted solution: Pipet 25 mL of the Sample solution into a 50-mL volumetric flask. Cool to 20°, and dilute with water to volume at 20°. Maintain a temperature of 20° for 30 min.

Acid-inverted solution: Pipet 25 mL of the Sample solution into a 50-mL volumetric flask. Slowly add 6 mL of dilute hydrochloric acid (1 in 2) while rotating it, dilute with water nearly to volume, and mix. Place the flask in a water bath maintained at a temperature of 60°, continuously shake the flask in the bath for 3 min, and allow the flask to remain in the bath for a total of 10 min. Immediately cool to 20° by plunging the flask into a cold bath, and dilute with water to volume at 20°. Maintain the flask at a temperature of 20° for 30 min.

Determine the specific rotation of the Uninverted solution and Acid-inverted solution at 20°.

Acceptance criteria

The specific rotation determined from the Uninverted solution: 62.6°-73.4°

The specific rotation determined from the Acid-inverted solution: Levorotatory

MICROBIAL ENUMERATION TESTS (61) and TESTS FOR SPECIFIED MICROORGANISMS (62): The total aerobic microbial count does not exceed 10³ cfu/g, and

the total combined molds and yeasts count does not exceed 10₂ cfu/g. It meets the requirements of the tests for the absence of Salmonella species and Escherichia coli.

LOSS ON DRYING (731)

Analysis: Dry at 105° for 4 h.

Acceptance criteria: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in well-closed containers.

LABELING: Label it to indicate the name and amount of any added lubricant.

USP REFERENCE STANDARDS (11)

USP Anhydrous Lactose RS

USP Compressible Sugar RS

USP Dextrose RS

USP Fructose RS

USP Maltose Monohydrate RS

USP Sucrose RS