Sucrose octadecanoate [25168-73-4].
Sucrose Stearate is a mixture of sucrose esters, mainly sucrose stearate, obtained by transesterification of stearic acid methyl esters derived from vegetable origin with sucrose. The manufacture of the fatty acid methyl esters includes a distillation step. The mono- and diesters requirements differ for the two types of sucrose stearate as set forth in the following table.
• A. It meets the requirements of the Fatty Acid Composition test.
• B. It meets the requirements of Content of Monoesters, Diesters, Triesters, and Polyesters.
• Content of Monoesters, Diesters, Triesters, and Polyesters
Mobile phase: Tetrahydrofuran
Sample solution: 15 mg/mL of Sucrose Stearate in tetrahydrofuran
Mode: LC, size-exclusion
Detector: Differential refractometer
Column: 7-mm × 60-cm; packing L21, 100 . [NoteTwo 7-mm × 30-cm L21 columns may be used in place of one 60-cm column, provided system suitability requirements are met. ]
Flow rate: 1.2 mL/min
Injection size: 20 µL
Sample: Sample solution
[NoteThe relative retention time with reference to the monoester peak (retention time is approximately 10 min) is about 0.92 for diesters, and about 0.90 for triesters and polyesters. ]
[NoteDisregard solvent peaks and peaks having a signal-to-noise ratio less than 10. ]
Calculate the percentage of monoesters in the portion of Sucrose Stearate taken:
Result = A × (100 D S E)/100
Calculate the percentage of diesters in the portion of Sucrose Stearate taken:
Result = B × (100 D S E)/100
Calculate the percentage of triesters and polyesters in the portion of Sucrose Stearate taken:
Result = C × (100 D S E)/100
• Fatty Acid Composition: Sucrose Stearate exhibits the following composition profiles of fatty acids, as determined in Fats and Fixed Oils 401, Fatty Acid Composition.
• Fats and Fixed Oils, Acid Value 401: NMT 6, determined on a 3-g sample. Use a freshly neutralized mixture of 2-propanol and water (2:1), and gently heat.
• Procedure: Free Sucrose
Solution A: 10 µg/mL of ammonium acetate in acetonitrile
Solution B: 10 µg/mL of ammonium acetate in tetrahydrofuran and water (90:10)
Diluent: Tetrahydrofuran and water (87.5:12.5)
System suitability solution: 10 µg/mL of USP Sucrose RS in Diluent
Standard solutions: 0.50, 1.0, 2.0, and 2.5 mg/mL of USP Sucrose RS in Diluent
Sample solution: 50 mg/mL of Sucrose Stearate in Diluent
Detector: Evaporative light-scattering. [NoteIf the detector has different setting parameters, adjust the detector settings so as to comply with the System Suitability requirements. ]
Carrier gas: Nitrogen
Detector temperature: 45
Nebulizer temperature: 40
Column: 4.6-mm × 0.25-m; packing L8
Injection size: 20 µL
Mobile phase and flow rate: See the gradient table below.
Sample: System suitability solution
[NoteThe retention time for sucrose stearate is about 26 min. ]
Signal-to-noise ratio: 10:1
Samples: Standard solutions and Sample solution
Prepare a standard curve by plotting the peak response versus concentration of sucrose in the Standard solution. Calculate the quantity of free sucrose in the Sucrose Stearate taken.
Acceptance criteria: NMT 4.0%
• Water Determination, Method Ia 921: NMT 4.0%, on a 0.20-g sample
• Total Ash
Analysis: Heat a silica or platinum crucible to redness for 30 min, allow to cool in a desiccator, and weigh. Transfer a 1.0-g sample into a crucible. Dry at 100105 for 1 h and ignite to constant weight in a muffle furnace at 600 ± 25, allowing the crucible to cool in a desiccator after each ignition. Flames should not be produced at any time during the procedure. If after prolonged ignition the ash still contains black particles, add hot water, pass through an ashless filter paper, and ignite the residue and the filter paper. Combine the filtrate with the ash, carefully evaporate to dryness, and ignite to constant weight.
Acceptance criteria: NMT 1.5%
• Labeling: Label to indicate whether it is Type I or Type II.
• Packaging and Storage: Preserve in a well-closed container. Protect from humidity and avoid high temperatures.
• USP Reference Standards 11
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USP35NF30 Page 1998Pharmacopeial Forum: Volume No. 35(2) Page 328