Acebutolol Hydrochloride Capsules
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This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition
Issued and maintained by the United States Pharmacopeial Convention (USP)
1 DEFINITION
Acebutolol Hydrochloride Capsules contain the equivalent of NLT 90.0% and NMT 110.0% of the labeled amount of acebutolol (C18H28N2O4).
2 IDENTIFICATION
A. The UV absorption spectra of the major peak of the Sample solution exhibit maxima and minima at the same wavelengths as those of the corresponding peak of the Standard solution, as obtained in the Assay.
B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
3 ASSAY
3.1 PROCEDURE
Buffer: Dissolve 2.4 g of sodium 1-decanesulfonate in 1000 mL of water. Adjust with glacial acetic acid to a pH of 3.5.
Mobile phase: Methanol and Buffer (60:40)
Standard solution: 0.22 mg/mL of USP Acebutolol Hydrochloride RS in methanol. [NOTE-This is equivalent to 0.2 mg/mL of acebutolol.]
Sample stock solution: Nominally 1 mg/mL of acebutolol prepared as follows. Transfer an equivalent to 200 mg of acebutolol, from the contents of NLT 20 Capsules, to a 200-mL volumetric flask. Add 180 mL of methanol, and stir by mechanical means for 30 min. Dilute with methanol to volume.
Sample solution: Nominally 0.2 mg/mL of acebutolol in methanol from Sample stock solution
Chromatographic system
(See Chromatography (621), System Suitability.)
Mode: LC
Detector: UV 254 nm. For Identification A, use a diode-array detector in the range of 200-400 nm.
Column: 3.9-mm x 15-cm; 4-µm packing L1
Flow rate: 1 mL/min
Injection volume: 20 µL
System suitability
Sample: Standard solution
Suitability requirements
Tailing factor: NMT 1.5
Relative standard deviation: NMT 2.0
3.2 Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of acebutolol (C18H28N2O4) in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = peak response of acebutolol from the Sample solution
rS = peak response of acebutolol from the Standard solution
CS = concentration of USP Acebutolol Hydrochloride RS in the Standard solution (mg/mL)
CU = nominal concentration of acebutolol from the Sample solution (mg/mL)
Mr1 = molecular weight of acebutolol, 336.43
Mr2 = molecular weight of acebutolol hydrochloride, 372.89
Acceptance criteria: 90.0%-110.0%
4 PERFORMANCE TESTS
4.1 DISSOLUTION (711)
Medium: Water; 900 mL
Apparatus 2: 50 rpm
Time: 30 min
Standard solution: A known concentration of USP Acebutolol Hydrochloride RS in Medium
Sample solution: Pass a portion of the solution under test through a suitable filter.
Instrumental conditions
(See Ultraviolet-Visible Spectroscopy (857).)
Mode: UV
Analytical wavelength: 232 nm
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of acebutolol (C18H28N2O4) dissolved:
(AU/AS) x CS x V x (1/L) x (Mr1/Mr2) x 100
AU = absorbance of the Sample solution
AS = absorbance of the Standard solution
CS = concentration of acebutolol in the Standard solution (mg/mL)
V = volume of Medium, 900 mL
L = label claim (mg/Tablet)
Mr1 = molecular weight of acebutolol, 336.43
Mr2 = molecular weight of acebutolol hydrochloride, 372.89
Tolerances: NLT 80% (Q) of the labeled amount of acebutolol (C18H28N2O4) is dissolved.
4.2 UNIFORMITY OF DOSAGE UNITS (905)
Meet the requirements
5 IMPURITIES
5.1 ORGANIC IMPURITIES
5.1.1 Test 1
Buffer: Prepare as directed in the Assay.
Mobile phase: Methanol and Buffer (44:56)
Diluent: Methanol and Buffer (50:50)
Standard stock solution: 0.6 mg/mL of USP Acebutolol Hydrochloride RS prepared as follows. To a suitable amount of USP Acebutolol Hydrochloride RS in a suitable volumetric flask, add methanol, about 24% of the flask volume, swirl to dissolve, and dilute with Diluent to volume.
Standard solution: 1.4 µg/mL of USP Acebutolol Hydrochloride RS in Diluent from Standard stock solution
Sample stock solution: Nominally 2.5 mg/mL of acebutolol prepared as follows. Transfer a portion of the contents of 20 opened Capsules, equivalent to 250 mg of acebutolol, to a 100-mL volumetric flask. Add 25 mL of methanol and shake by mechanical means for 15 min.
Dilute with Diluent to volume. Centrifuge a portion of this solution and use the supernatant.
Sample solution: Nominally 250 µg/mL of acebutolol in Diluent from Sample stock solution
Chromatographic system
(See Chromatography (621), System Suitability.)
Mode: LC
Detector: UV 240 nm
Column: 3.9-mm x 15-cm; 4-um packing L1
Flow rate: 1 mL/min
Injection volume: 35 µL
Run time: NLT 2 times the retention time of acebutolol
System suitability
Sample: Standard solution
Suitability requirements
Relative standard deviation: NMT 6.0%
Analysis
Samples: Diluent, Standard solution, and Sample solution
Calculate the percentage of each impurity eluting before the acebutolol peak in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = peak response of each individual impurity from the Sample solution
rS = peak response of acebutolol from the Standard solution
CS = concentration of USP Acebutolol Hydrochloride RS in the Standard solution (µg/mL)
CU = nominal concentration of acebutolol in the Sample solution (µg/mL)
Mr1 = molecular weight of acebutolol, 336.43
Mr2 = molecular weight of acebutolol hydrochloride, 372.89
Acceptance criteria: NMT 0.5% of any individual impurity. Disregard any peaks from the Diluent.
5.1.2 Test 2
Buffer and System suitability: Proceed as directed in Test 1.
Mobile phase: Methanol and Buffer (50:50)
Standard stock solution: 0.6 mg/mL of USP Acebutolol Hydrochloride RS prepared as follows. To a suitable amount of USP Acebutolol Hydrochloride RS in a suitable volumetric flask, add methanol, about 24% of the flask volume, swirl to dissolve, and dilute with Mobile phase to volume.
Standard solution: 1.4 µg/mL of USP Acebutolol Hydrochloride RS in Mobile phase from Standard stock solution
Sample stock solution: Nominally 2.5 mg/mL of acebutolol prepared as follows. Transfer a portion of the contents of 20 opened Capsules, equivalent to 250 mg of acebutolol, to a 100-mL volumetric flask. Add 25 mL of methanol and shake by mechanical means for 15 min. Dilute with Mobile phase to volume.
Sample solution: Nominally 250 µg/mL of acebutolol in Diluent from Sample stock solution prepared as follows. Centrifuge a portion of Sample stock solution, and transfer 10.0 mL of the clear supernatant to a 100-mL volumetric flask. Dilute with Mobile phase to volume.
Chromatographic system
(See Chromatography (621), System Suitability.)
Proceed as directed in Test 1 except for the Injection volume and Run time.
Injection volume: 70 µL
Run time: NLT 3 times the retention time of acebutolol
Analysis
Samples: Mobile phase, Standard solution, and Sample solution
Calculate the percentage of each impurity eluting after the acebutolol peak in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
rU = peak response of each individual impurity from the Sample solution
rS = peak response of acebutolol from the Standard solution
CS = concentration of USP Acebutolol Hydrochloride RS in the Standard solution (µg/mL)
CU = nominal concentration of acebutolol in the Sample solution (µg/mL)
Mr1 = molecular weight of acebutolol, 336.43
Mr2 = molecular weight of acebutolol hydrochloride, 372.89
Acceptance criteria
Test 2: NMT 0.5% of any individual impurity. Disregard any peaks from the Mobile phase.
Sum of impurities from Test 1 and Test 2: NMT 1.0%
6 ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in tight containers, and store at controlled room temperature.
USP REFERENCE STANDARDS (11)
USP Acebutolol Hydrochloride RS
