Printed on: Wed Aug 04 2021, 06:22:39 PM Official Status: Currently Official on 04-Aug-2021 DocId: 1_GUID-443A9951-3E44-46EC-A62B-2C0963DD591C_4_en-US

(EST)
Printed by: Le Tran Official Date: Official as of 01-May-2020 Document Type: NF @2021 USPC
1

IMPURITIES
Sucralose • RESIDUE ON IGNITION á281ñ: NMT 0.7%
• LIMIT OF METHANOL
Internal standard solution: 0.1 µL/mL of n-propyl alcohol
in pyridine
Standard solution: 0.2 µL/mL of methanol in Internal
standard solution
Sample solution: 0.2 g/mL of Sucralose in Internal standard
solution
Chromatographic system
(See Chromatography á621ñ, System Suitability.)
Mode: GC
Detector: Flame ionization
Column: 4-mm × 2-m glass column; packed with 80- to
100-mesh silanized support S6
C12H19Cl3O8 397.63 Temperature
1,6-Dichloro-1,6-dideoxy-β-D-fructofuranosyl-4-chloro-4- Column: 150°
deoxy-α-D-galactopyranoside; Detector: 250°
1′,4,6′-Trichlorogalactosucrose [56038-13-2]. Injector: 200°
Carrier gas: Helium
DEFINITION
Flow rate: 20 mL/min
Sucralose contains NLT 98.0% and NMT 102.0%
Injection size: 1 µL
of C12H19Cl3O8, calculated on the anhydrous basis.

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System suitability
IDENTIFICATION Sample: Standard solution
Suitability requirements
Change to read: Relative standard deviation: NMT 2.0%
Analysis
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared ci Samples: Standard solution and Sample solution
Spectroscopy: 197K▲ (CN 1-May-2020) Calculate the percentage of methanol in the portion of
• B. The retention time of the principal peak of the Sample Sucralose taken:
solution corresponds to that of the Standard solution, as
obtained in the Assay. Result = (R U/R S) × [(C S/C U) × F 1] × F 2 × 100
• C. The R F value of the principal spot of the Sample solution
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corresponds to that of Standard solution A, as obtained in RU = peak response ratio of methanol to n-propyl
the test for Related Compounds. alcohol, from the Sample solution
RS = peak response ratio of methanol to n-propyl
ASSAY alcohol, from the Standard solution
• PROCEDURE CS = concentration of methanol in the Standard
Mobile phase: Acetonitrile and water (3:17) solution (µL/mL)
Standard solution: 1 mg/mL of USP Sucralose RS in Mobile
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CU = concentration of Sucralose in the Sample solution

phase (g/mL)
Sample solution: 1 mg/mL of Sucralose in Mobile phase F1 = conversion factor from µL to mL
Chromatographic system
(See Chromatography á621ñ, System Suitability.) F2 = specific gravity of methanol, 0.79 g/cm3
Mode: LC
Detector: Refractive index Acceptance criteria: NMT 0.1%
Column: 8-mm × 10-cm; packing L1 • RELATED COMPOUNDS
Flow rate: 1.5 mL/min Adsorbent: 0.20-mm layer of octadecylsilanized
Injection size: 20 µL chromatographic silica gel. The thin-layer chromatographic
System suitability plate also has a preadsorbent zone.
Sample: Standard solution Detection reagent: Sulfuric acid in methanol (3 in 20)
[NOTE—The retention time of sucralose is about 9 min.] Standard solution A: 10.0 mg/mL of USP Sucralose RS in
Suitability requirements methanol
Relative standard deviation: NMT 2.0% Standard solution B: 0.5 mL Standard solution A diluted to
Analysis 10.0 mL with methanol
Samples: Standard solution and Sample solution Sample solution: 100.0 mg/mL of Sucralose in methanol
Calculate the percentage of sucralose (C12H19Cl3O8) in the Developing solvent system: Acetonitrile and sodium
chloride solution (1 in 20) (3:7)
portion of Sucralose taken:
Application volume: 5 µL
Result = (r U/r S) × (C S/C U) × 100 Analysis
Samples: Standard solution A, Standard solution B, and
rU = peak response of the Sample solution Sample solution
rS = peak response of the Standard solution Proceed as directed under Chromatography á621ñ,
Thin-Layer Chromatography. Spray the plate with Detection
CS = concentration of USP Sucralose RS in the Standard
reagent. Heat the plate for 10 min at 125°.
solution (mg/mL)
Acceptance criteria: The R F value of the principal spot from
CU = concentration of Sucralose in the Sample solution
(mg/mL) the Sample solution corresponds to that obtained from
Standard solution A, and the color of any other single spot
Acceptance criteria: 98.0%–102.0% on the anhydrous from the Sample solution is not more intense than that of
basis the principal spot from Standard solution B (0.5%).

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Printed on: Wed Aug 04 2021, 06:22:39 PM Official Status: Currently Official on 04-Aug-2021 DocId: 1_GUID-443A9951-3E44-46EC-A62B-2C0963DD591C_4_en-US
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Printed by: Le Tran Official Date: Official as of 01-May-2020 Document Type: NF @2021 USPC
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• LIMIT OF HYDROLYSIS PRODUCTS reagent, and heat the plate at 100 ± 2° for 15 min. If the
[NOTE—This test does not require a developing spot from Standard solution A has darkened, repeat the
solvent.] test, heating for a shorter period of time. Immediately
Adsorbent: 0.25-mm layer of chromatographic silica gel after heating, view the plate against a dark background.
Spray reagent: 12.3 mg/mL of p-anisidine and 16.6 mg/mL Acceptance criteria: The color of the spot from the Sample
of phthalic acid in methanol. Store the solution in the dark solution is not more intense than that from Standard solution
and refrigerate to prevent discoloration. Discard if the B (0.1%).
solution becomes discolored. [CAUTION—p-Anisidine is toxic
if inhaled or if absorbed through the skin.] SPECIFIC TESTS
Standard solution A: 100 mg/mL of mannitol • OPTICAL ROTATION, Specific Rotation á781Sñ: +84.0° to
Standard solution B: 0.4 mg/mL of fructose and +87.5° at 20°
100 mg/mL of mannitol Sample solution: 10 mg/mL of Sucralose
Sample solution: 250 mg/mL of Sucralose in methanol • WATER DETERMINATION, Method I á921ñ: NMT 2.0%
Application volume: 5-µL portions separately applied in ADDITIONAL REQUIREMENTS
1-µL increments, allowing the plate to dry between • PACKAGING AND STORAGE: Preserve in well-closed
applications containers, in a cool, dry place, at a temperature not
Analysis exceeding 21°.
Samples: Standard solution and Sample solution • USP REFERENCE STANDARDS á11ñ
Proceed as directed under Chromatography á621ñ, USP Sucralose RS
Thin-Layer Chromatography. Spray the plate with Spray

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