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Printed by: Nguyen Nhan Official Date: Official as of 01-May-2020 Document Type: USP @2021 USPC
1

rU = peak response from the Sample solution

Acarbose rS = peak response from the Standard solution
CS = concentration of USP Acarbose RS in the Standard
solution (mg/mL)
CU = concentration of the Sample solution (mg/mL)

Acceptance criteria: 95.0%–102.0% on the anhydrous

basis
IMPURITIES
• RESIDUE ON IGNITION á281ñ
C25H43NO18 645.60 Sample: 1.0 g
D-Glucose, O-4,6-dideoxy-4-[[[1S-(1α,4α,5β,6α)]-4,5,6- Acceptance criteria: NMT 0.2%
trihydroxy-3-(hydroxymethyl)-2-cyclohexen-1-yl]amino]-α- • CHROMATOGRAPHIC PURITY
D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-; Mobile phase, System suitability solution, Sample
O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- solution, and Chromatographic system: Proceed as
(hydroxymethyl)-2-cyclohexen-1-yl]amino}-α-D- directed in the Assay.
glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-D- Diluted sample solution: Dilute 1.0 mL of the Sample
glucose [56180-94-0]. solution with water to 100.0 mL.
Analysis
DEFINITION
Samples: Sample solution and Diluted sample solution
Acarbose is produced by certain strains of Actinoplanes
Calculate the percentage of each impurity in the portion of
utahensis. It contains NLT 95.0% and NMT 102.0% of
Acarbose taken:

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acarbose (C25H43NO18), calculated on the anhydrous basis.
IDENTIFICATION Result = (r U/r A) × (1/F) × 100

Change to read: rU = peak response of each impurity from the Sample

ci solution
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared rA = peak response of the main acarbose peak from
Spectroscopy: 197K▲ (CN 1-May-2020) the Diluted sample solution
• B. The retention time of the major peak of the Sample F = relative response factor for each impurity (see
solution corresponds to that of the Standard solution, as Table 1)
obtained in the Assay.
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ASSAY Acceptance criteria: See Table 1.
• PROCEDURE
Table 1
Solution A: 0.6 mg/mL of monobasic potassium phosphate
and 0.35 mg/mL of dibasic sodium phosphate in water Relative Relative Acceptance
Retention Response Criteria,
Mobile phase: Acetonitrile and Solution A (3:1) Name Time Factor NMT (%)
System suitability solution: 20 mg/mL of USP Acarbose
O

System Suitability Mixture RS in water Impurity Aa 0.9 1 0.6

Standard solution: 20 mg/mL of USP Acarbose RS in water Impurity Bb 0.8 1.6 0.5
Sample solution: 20 mg/mL of Acarbose in water
Chromatographic system Impurity C c
1.2 1 1.5
(See Chromatography á621ñ, System Suitability.) Impurity D d
0.5 1.33 1.0
Mode: LC
Detector: UV 210 nm Impurity Ee 1.7 0.8 0.2
Column: 4-mm × 25-cm; packing L8 Impurity Ff
1.9 0.8 0.3
Column temperature: 35°
Flow rate: 2 mL/min Impurity Gg 2.2 0.8 0.3
Injection volume: 10 µL Impurity Hh 0.6 1 0.2
System suitability
Sample: System suitability solution Any individual
unknown impur- — —
Identify the acarbose peak and the peaks due to the ity 0.2
impurities listed in Table 1.
Suitability requirements Total impurities — — 3.0
Peak-to-valley ratio: The ratio of the height of the a O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl)
impurity A peak to the height of the valley between the cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-
impurity A peak and the acarbose peak is NLT 1.2. (1→4)-D-arabino-hex-2-ulopyranose.
Chromatogram comparability: The chromatogram b (1R,4R,5S,6R)-4,5,6-Trihydroxy-2-(hydroxymethyl)cyclohex-2-enyl 4-O-[4,6-
obtained is similar to the chromatogram provided with dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl)cyclohex-2-
USP Acarbose System Suitability Mixture RS for the enyl]amino}-α-D-glucopyranosyl]-α-D-glucopyranoside.
c α-D-Glucopyranosyl 4-O-[4,6-dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-
known impurities found.
(hydroxymethyl)cyclohex-2-enyl]amino}-α-D-glucopyranosyl]-α-D-
Analysis glucopyranoside.
Samples: Standard solution and Sample solution d 4-O-[4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl)
Calculate the percentage of acarbose (C25H43NO18) in the cyclohex-2-enyl]amino}-α-D-glucopyranosyl]-D-glucopyranose.
e O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl)
portion of Acarbose taken:
cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-
(1→4)-O-α-D-glucopyranosyl-(1→4)-D-arabino-hex-2-ulopyranose (4-O-α-
Result = (r U/r S) × (C S/C U) × 100 acarbosyl-D-fructopyranose).

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f O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl) Acceptance criteria: +168° to +183°

cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl- • PH á791ñ
(1→4)-O-α-D-glucopyranosyl-(1→4)-D-glucopyranose (4-O-α-acarbosyl-D-
glucopyranose). Sample solution: 50 mg/mL
g α-D-Glucopyranosyl O-4,6-dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- Acceptance criteria: 5.5–7.5
(hydroxymethyl)cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-α-D- • WATER DETERMINATION, Method Ic á921ñ : NMT 4.0%
glucopyranosyl-(1→4)-O-α-D-glucopyranoside (α-D-glucopyranosyl α-
acarboside). ADDITIONAL REQUIREMENTS
h O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl) • PACKAGING AND STORAGE: Preserve in tight containers.
cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-6-deoxy-α-D- • USP REFERENCE STANDARDS á11ñ
glucopyranosyl-(1→4)-D-glucopyranose.
USP Acarbose RS
USP Acarbose System Suitability Mixture RS
SPECIFIC TESTS
• OPTICAL ROTATION, Specific Rotation á781Sñ
Sample solution: 10 mg/mL in water

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