Printed on: Fri Jan 05 2024, 09:08:40 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-A4C261F9-BA9C-46C9-9FDA-9B3301067158_2_en-US
Printed by: USP NF Official Date: Official as of 01-Aug-2019 Document Type: USP @2024 USPC
Do Not Distribute DOI Ref: o26u4 DOI: https://doi.org/10.31003/USPNF_M8408_02_01
1
Add the following: CS = concentration of USP Benzphetamine
Hydrochloride RS in the Standard solution
(mg/mL)
▲
Benzphetamine Hydrochloride Tablets CU = nominal concentration of benzphetamine
hydrochloride in the Sample solution (mg/mL)
DEFINITION
Benzphetamine Hydrochloride Tablets contain NLT 93.0%
Acceptance criteria: 93.0%–105.0%
and NMT 105.0% of the labeled amount of benzphetamine
hydrochloride (C17H21N · HCl). PERFORMANCE TESTS
• DISSOLUTION á711ñ
IDENTIFICATION Use plastic vials for analysis.
• A. The retention time of the benzphetamine peak of the Medium: Water; 900 mL
Sample solution corresponds to that of the Standard Apparatus 2: 50 rpm
solution, as obtained in the Assay. Time: 30 min
• B. The UV spectrum of the benzphetamine peak of the Buffer: Dissolve 2.76 g of monobasic sodium phosphate
Sample solution corresponds to that of the Standard dihydrate in 1000 mL of water. Add 0.5 mL of triethylamine
solution, as obtained in the Assay. and adjust with phosphoric acid to a pH of 6.0.
ASSAY Mobile phase: Acetonitrile and Buffer (70:30)
• PROCEDURE Standard stock solution: 0.55 mg/mL of USP
Buffer: Dissolve 2.76 g of monobasic sodium phosphate Benzphetamine Hydrochloride RS, prepared as follows.
dihydrate in 1000 mL of water. Add 1.0 mL of triethylamine Transfer an adequate amount of USP Benzphetamine
and adjust with phosphoric acid to a pH of 4.5. Hydrochloride RS to a suitable volumetric flask. Add 5% of
Solution A: Acetonitrile and Buffer (10:90) the final volume of acetonitrile and sonicate to dissolve.
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Solution B: Acetonitrile and water (80:20) Dilute with Medium to volume.
Mobile phase: Solution A and Solution B (65:35) Standard solution: 0.055 mg/mL of USP Benzphetamine
Diluent: Methanol and water (50:50) Hydrochloride RS in Medium from Standard stock solution
Standard solution: 0.2 mg/mL of USP Benzphetamine Sample solution: Pass a portion of the solution under test
Hydrochloride RS in Diluent. Sonicate to dissolve if
ci through a suitable filter of 0.45-µm pore size.
necessary. Chromatographic system
Sample solution: Nominally 0.2 mg/mL of benzphetamine (See Chromatography á621ñ, System Suitability.)
hydrochloride in Diluent, prepared as follows. Transfer an Mode: LC
adequate amount of benzphetamine hydrochloride from Detector: UV 207 nm
NLT 20 finely powdered Tablets to a suitable volumetric Column: 4.6-mm × 25-cm; 5-µm packing L7
ffi
flask. Add about 60% of the final volume of Diluent and Column temperature: 25°
shake vigorously to disperse the Tablet powder. Sonicate Flow rate: 1.0 mL/min
for an additional NLT 60 min with intermediate shaking. Injection volume: 10 µL
Cool to room temperature and dilute with Diluent to Run time: NLT 1.8 times the retention time of
volume. Pass a portion through a suitable filter with a benzphetamine
0.45-µm pore size. Discard the first few milliliters of filtrate. System suitability
O
Chromatographic system Sample: Standard solution
(See Chromatography á621ñ, System Suitability.) Suitability requirements
Mode: LC Tailing factor: NMT 2.0
Detector: UV 207 nm. For Identification B, use a diode array Relative standard deviation: NMT 2.0%
detector in the range of 200–400 nm. Analysis
Column: 4.6-mm × 25-cm; 5-µm packing L7 Samples: Standard solution and Sample solution
Temperatures Calculate the percentage of the labeled amount of
Autosampler: 15° benzphetamine hydrochloride (C17H21N · HCl) dissolved:
Column: 40°
Flow rate: 1.0 mL/min Result = (rU/rS) × CS × V × (1/L) × 100
Injection volume: 10 µL
Run time: NLT 2.1 times the retention time of rU = peak response of benzphetamine from the
benzphetamine Sample solution
System suitability rS = peak response of benzphetamine from the
Sample: Standard solution Standard solution
Suitability requirements CS = concentration of USP Benzphetamine
Tailing factor: NMT 2.0 Hydrochloride RS in the Standard solution
Relative standard deviation: NMT 2.0% (mg/mL)
Analysis V = volume of Medium (mL), 900
Samples: Standard solution and Sample solution L = label claim (mg/Tablet)
Calculate the percentage of the labeled amount of
benzphetamine hydrochloride (C17H21N · HCl) in the Tolerances: NLT 80% (Q) of the labeled amount of
portion of Tablets taken: benzphetamine hydrochloride (C17H21N · HCl) is dissolved.
• UNIFORMITY OF DOSAGE UNITS á905ñ: Meet the
Result = (rU/rS) × (CS/CU) × 100 requirements
IMPURITIES
rU = peak response of benzphetamine from the • ORGANIC IMPURITIES
Sample solution Solution A: 1.38 g of monobasic sodium phosphate
rS = peak response of benzphetamine from the dihydrate in 1000 mL of water
Standard solution Solution B: Acetonitrile and water (80:20)
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Printed on: Fri Jan 05 2024, 09:08:40 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-A4C261F9-BA9C-46C9-9FDA-9B3301067158_2_en-US
Printed by: USP NF Official Date: Official as of 01-Aug-2019 Document Type: USP @2024 USPC
Do Not Distribute DOI Ref: o26u4 DOI: https://doi.org/10.31003/USPNF_M8408_02_01
2
Mobile phase: See Table 1. Relative standard deviation: NMT 5.0%, Standard
solution
Table 1 Signal-to-noise ratio: NLT 10, Sensitivity solution
Time Solution A Solution B Analysis
(min) (%) (%) Samples: Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of
0 80 20
Tablets taken:
5 75 25
Result = (rU/rS) × (CS/CU) × (1/F) × 100
10 60 40
15 40 60 rU = peak response of each impurity from the Sample
solution
20 15 85
rS = peak response of benzphetamine from the
22 15 85 Standard solution
CS = concentration of USP Benzphetamine
23 80 20
Hydrochloride RS in the Standard solution
30 80 20 (mg/mL)
CU = nominal concentration of benzphetamine
Diluent: Methanol and water (50:50) hydrochloride in the Sample solution (mg/mL)
System suitability solution: 0.002 mg/mL each of USP F = relative response factor of each individual
Benzphetamine Hydrochloride RS, USP Benzphetamine impurity (see Table 2)
Related Compound E RS, and USP Methamphetamine
Acceptance criteria: See Table 2.
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Hydrochloride RS in Diluent. Sonicate to dissolve if
necessary.
Table 2
Sensitivity solution: 0.0001 mg/mL of USP Benzphetamine
Hydrochloride RS in Diluent Relative Relative Acceptance
Standard solution: 0.002 mg/mL of USP Benzphetamine Retention Response Criteria,
Name Time Factor NMT (%)
Hydrochloride RS in Diluent. Sonicate to dissolve if
necessary.
Sample solution: Nominally 1 mg/mL of benzphetamine
hydrochloride in Diluent, prepared as follows. Transfer an
ci Methamphetamine
hydrochloride
Benzphetamine related
0.35 0.68 0.10
adequate amount of benzphetamine hydrochloride from compound E 0.90 0.93 0.10
NLT 20 finely powdered Tablets to a suitable volumetric
ffi
Benzphetamine
flask. Add about 40% of the final volume of Diluent and hydrochloride 1.00 1.00
—
shake vigorously to disperse the Tablet powder. Sonicate
for an additional NLT 60 min with intermediate shaking. Any unspecified
—
impurity 1.00 0.10
Cool to room temperature and dilute with Diluent to
volume. Pass a portion through a suitable filter with a Total impurities — — 1.0
0.45-µm pore size. Discard the first few milliliters of filtrate.
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Chromatographic system ADDITIONAL REQUIREMENTS
(See Chromatography á621ñ, System Suitability.) • PACKAGING AND STORAGE: Preserve in tight containers, and
Mode: LC store at controlled room temperature.
Detector: UV 207 nm • USP REFERENCE STANDARDS á11ñ
Column: 4.6-mm × 25-cm; 5-µm packing L1 USP Benzphetamine Hydrochloride RS
Temperatures USP Benzphetamine Related Compound E RS
Autosampler: 15° (1S,2S)-2-[Benzyl(methyl)amino]-1-phenylpropan-1-ol
Column: 40° hydrochloride.
Flow rate: 1.2 mL/min C17H21NO · HCl 291.82
Injection volume: 20 µL USP Methamphetamine Hydrochloride RS
System suitability (S)-N-Methyl-1-phenylpropan-2-amine hydrochloride.
Samples: System suitability solution, Sensitivity solution, and C10H15N · HCl 185.69▲ (USP 1-Aug-2019)
Standard solution
Suitability requirements
Resolution: NLT 3.0 between benzphetamine related
compound E and benzphetamine, System suitability
solution
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