Printed on: Wed Feb 08 2023, 11:19:28 PM(EST) Status: Currently Official on 09-Feb-2023 DocId: GUID-3ED89AF2-51AF-4471-BACE-94AD0510DE2A_4_en-US

Printed by: Dang Van Vu Official Date: Official as of 01-May-2020 Document Type: USP @2023 USPC
Do Not Distribute DOI Ref: r1txs DOI: https://doi.org/10.31003/USPNF_M115_04_01
1

CS = concentration of USP Acarbose RS in the Standard

Acarbose solution (mg/mL)
CU = concentration of the Sample solution (mg/mL)

Acceptance criteria: 95.0%–102.0% on the anhydrous

basis
IMPURITIES
C25H43NO18 645.60 • RESIDUE ON IGNITION á281ñ
D-Glucose, O-4,6-dideoxy-4-[[[1S-(1α,4α,5β,6α)]-4,5,6- Sample: 1.0 g
trihydroxy-3-(hydroxymethyl)-2-cyclohexen-1-yl]amino]-α- Acceptance criteria: NMT 0.2%
D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-; • CHROMATOGRAPHIC PURITY
O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- Mobile phase, System suitability solution, Sample
(hydroxymethyl)-2-cyclohexen-1-yl]amino}-α-D- solution, and Chromatographic system: Proceed as
glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-D- directed in the Assay.
glucose CAS RN®: 56180-94-0; UNII: T58MSI464G. Diluted sample solution: Dilute 1.0 mL of the Sample
solution with water to 100.0 mL.
DEFINITION Analysis
Acarbose is produced by certain strains of Actinoplanes Samples: Sample solution and Diluted sample solution
utahensis. It contains NLT 95.0% and NMT 102.0% of Calculate the percentage of each impurity in the portion of
acarbose (C25H43NO18), calculated on the anhydrous basis. Acarbose taken:
IDENTIFICATION Result = (r U/r A) × (1/F) × 100

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Change to read:
rU = peak response of each impurity from the Sample
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared solution
Spectroscopy: 197K▲ (CN 1-May-2020) rA = peak response of the main acarbose peak from
• B. The retention time of the major peak of the Sample
ci the Diluted sample solution
solution corresponds to that of the Standard solution, as F = relative response factor for each impurity (see
obtained in the Assay. Table 1)

ASSAY Acceptance criteria: See Table 1.

• PROCEDURE
Solution A: 0.6 mg/mL of monobasic potassium phosphate Table 1
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and 0.35 mg/mL of dibasic sodium phosphate in water Relative Relative Acceptance
Mobile phase: Acetonitrile and Solution A (3:1) Retention Response Criteria,
System suitability solution: 20 mg/mL of USP Acarbose Name Time Factor NMT (%)
System Suitability Mixture RS in water Impurity Aa 0.9 1 0.6
Standard solution: 20 mg/mL of USP Acarbose RS in water
Sample solution: 20 mg/mL of Acarbose in water Impurity Bb 0.8 1.6 0.5
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Chromatographic system Impurity Cc 1.2 1 1.5

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

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Printed on: Wed Feb 08 2023, 11:19:28 PM(EST) Status: Currently Official on 09-Feb-2023 DocId: GUID-3ED89AF2-51AF-4471-BACE-94AD0510DE2A_4_en-US
Printed by: Dang Van Vu Official Date: Official as of 01-May-2020 Document Type: USP @2023 USPC
Do Not Distribute DOI Ref: r1txs DOI: https://doi.org/10.31003/USPNF_M115_04_01
2

g α-D-Glucopyranosyl O-4,6-dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3- • PH á791ñ

(hydroxymethyl)cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-α-D- Sample solution: 50 mg/mL
glucopyranosyl-(1→4)-O-α-D-glucopyranoside (α-D-glucopyranosyl α-
acarboside). Acceptance criteria: 5.5–7.5
h O-4,6-Dideoxy-4-{[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl) • WATER DETERMINATION, Method Ic á921ñ : NMT 4.0%
cyclohex-2-enyl]amino}-α-D-glucopyranosyl-(1→4)-O-6-deoxy-α-D-
glucopyranosyl-(1→4)-D-glucopyranose. ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers.
SPECIFIC TESTS • USP REFERENCE STANDARDS á11ñ
• OPTICAL ROTATION, Specific Rotation á781Sñ USP Acarbose RS
Sample solution: 10 mg/mL in water USP Acarbose System Suitability Mixture RS
Acceptance criteria: +168° to +183°

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