Propoxyphene Hydrochloride Capsules
DEFINITION
Propoxyphene Hydrochloride Capsules contain NLT 92.5% and NMT 107.5% of the labeled amount of C22H29NO2·HCl.
IDENTIFICATION
[Note—Use the following solutions in the tests below. ]
Standard solution:
Transfer 125 mg of USP Propoxyphene Hydrochloride RS to a 125-mL separator containing 8 mL of acetone, 32 mL of water, and 20 mL of 100 mg/mL of sodium carbonate solution, and swirl the mixture for 3 min. Add 25.0 mL of chloroform, insert the stopper, and shake the mixture by mechanical means for 1 h. Filter the chloroform extract through a layer of anhydrous sodium sulfate into a suitable beaker.
Sample solution:
Transfer a quantity of Capsule contents, remaining from the preparation of the Sample solution in the Assay, equivalent to 320 mg of propoxyphene hydrochloride to a 100-mL volumetric flask. Add 20 mL of acetone, and sonicate for 1 min. Dilute the solution with water to 100 mL. Allow to stand until the excipients have settled, usually 15–20 min. Transfer 40.0 mL of this solution to a 125-mL separator containing 20 mL of 100 mg/mL of sodium carbonate solution, and swirl the mixture for 3 min. Add 25.0 mL of chloroform, insert the stopper, and shake the mixture by mechanical means for 1 h. Filter the chloroform extract through a layer of anhydrous sodium sulfate into a suitable beaker. Use the Standard solution and the Sample solution for the following tests.
• A.
The IR absorption spectrum of the Sample solution, concentrated if necessary by evaporating a portion on a steam bath with the aid of a current of air to one-fifth of its volume, exhibits maxima only at the same wavelengths as that of the Standard solution.
• B.
The chromatogram of the Sample solution obtained as directed in the Assay exhibits a major peak for propoxyphene hydrochloride, the retention time of which corresponds to that exhibited for the Standard solution in the Assay.
ASSAY
• Procedure
Solution A:
6.8 g of monobasic potassium phosphate in 900 mL of water. Add 2.0 mL of triethylamine and adjust by the addition of phosphoric acid to a pH of 3.0 ± 0.1. Dilute with water to 1000 mL (phosphate buffer).
Diluent:
Acetonitrile and water (2:3)
Mobile phase:
Acetonitrile and Solution A (2:3)
Standard solution:
6.5 µg/mL of USP Propoxyphene Hydrochloride RS in Diluent. [Note—Sonicate as needed to aid dissolution. ]
Sample stock solution:
Remove, as completely as possible, the contents of NLT 20 Capsules. Weigh the contents, and determine the average weight/Capsule. Transfer mixed combined contents of Capsules nominally equivalent to 65 mg of propoxyphene hydrochloride to 50 mL of Diluent, sonicate for 5 min, and shake by mechanical means for 15 min. Dilute with Diluent to 200 mL, and filter, discarding the first 20 mL of the filtrate.
Sample solution:
Nominally equivalent to 6.5 µg/mL from the Sample stock solution diluted with Diluent
Chromatographic system
Mode:
LC
Detector:
UV 220 nm
Column:
4.6-mm × 3.3-cm; 3-µm packing L1 that is base-deactivated. [Note—Precondition the column for at least 30 min with Mobile phase. ]
Flow rate:
1 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 2 for the propoxyphene hydrochloride peak
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C22H29NO2·HCl in the portion of Capsules taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of USP Propoxyphene Hydrochloride RS in the Standard solution (µg/mL) |
| CU | = | = nominal concentration of propoxyphene hydrochloride in the Sample solution (µg/mL) |
Acceptance criteria:
92.5%–107.5%
PERFORMANCE TESTS
• Dissolution 
711
711
pH 4.5 acetate buffer:
2.99 g of sodium acetate trihydrate in 200 mL of water. Add 1.66 mL of glacial acetic acid, and dilute with water to 1000 mL.
Medium:
pH 4.5 acetate buffer; 500 mL
Apparatus 1:
100 rpm
Time:
60 min
Diluent:
Proceed as directed in the Assay.
Standard solution:
USP Propoxyphene Hydrochloride RS in Diluent
Sample solution:
Pass a portion of the solution under test through a suitable filter. Dilute with Diluent to a concentration that is similar to the Standard solution.
Analysis:
Proceed as directed in the Assay.
Tolerances:
NLT 85% (Q) of the labeled amount of C22H29NO2·HCl is dissolved.
• Uniformity of Dosage Units 905:
Meet the requirements
905:
Meet the requirements
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight containers.
• USP Reference Standards 11
11
USP Propoxyphene Hydrochloride RS 
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Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Clydewyn M. Anthony, Ph.D.
Senior Scientific Liaison 1-301-816-8139 |
(SM22010) Monographs - Small Molecules 2 |
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison 1-301-816-8106 |
(GCDF2010) General Chapters - Dosage Forms |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 4454
Pharmacopeial Forum: Volume No. 35(3) Page 574