Propoxyphene Hydrochloride and Acetaminophen Tablets
» Propoxyphene Hydrochloride and Acetaminophen Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amounts of propoxyphene hydrochloride (C22H29NO2·HCl) and acetaminophen (C8H9NO2).
Packaging and storage—
Preserve in tight containers.
Identification—
Transfer 1 finely ground Tablet to a test tube. If the Tablets are coated, first immerse the Tablet in acetone for 1½ minutes, remove the shell, and grind. Add 5 mL of methanol, shake for 5 minutes, and centrifuge. Use the clear supernatant as the Test solution. Prepare a Standard solution in methanol containing, in each mL, 130 mg of USP Acetaminophen RS and 13 mg of USP Propoxyphene Hydrochloride RS. Apply 5 µL of the Test solution on a line parallel to and about 2 cm from the bottom edge of a 20- × 5-cm thin-layer chromatographic plate (see Chromatography 
621
) coated with chromatographic silica gel mixture, and apply 5 µL of the Standard solution separately on the starting line. Place the plate in a developing chamber containing a mixture of butyl acetate, chloroform, and formic acid (60:40:20), and develop the chromatogram until the solvent front has moved about 15 cm above the line of application. Remove the plate, allow to dry in a hood, and view under short-wavelength UV light: the RF value of the principal spot from the Test solution corresponds to that from the Standard solution. Spray the plate with iodoplatinate TS: the RF value of the orange-brown spot from the Test solution corresponds to that from the Standard solution.
621) coated with chromatographic silica gel mixture, and apply 5 µL of the Standard solution separately on the starting line. Place the plate in a developing chamber containing a mixture of butyl acetate, chloroform, and formic acid (60:40:20), and develop the chromatogram until the solvent front has moved about 15 cm above the line of application. Remove the plate, allow to dry in a hood, and view under short-wavelength UV light: the RF value of the principal spot from the Test solution corresponds to that from the Standard solution. Spray the plate with iodoplatinate TS: the RF value of the orange-brown spot from the Test solution corresponds to that from the Standard solution.
Dissolution, Procedure for a Pooled Sample 711—
711—
Medium: pH 4.5 acetate buffer,
prepared as directed in the test for Dissolution under Propoxyphene Hydrochloride, Aspirin and Caffeine Capsules; 700 mL.
Apparatus 2:
50 rpm.
Time:
30 minutes.
Procedure—
Proceed as directed in the Assay, using a filtered portion of the solution under test, diluted with Mobile phase, and a Standard solution having accurately known concentrations of USP Propoxyphene Hydrochloride RS and USP Acetaminophen RS in Mobile phase. Calculate the amounts of propoxyphene hydrochloride (C22H29NO2·HCl) and acetaminophen (C8H9NO2) dissolved.
Tolerances—
Not less than 80% (Q) of the labeled amount of C22H29NO2·HCl and not less than 80% (Q) of the labeled amount of C8H9NO2 are dissolved in 30 minutes.
Uniformity of dosage units 905:
meet the requirements for Content Uniformity with respect to propoxyphene hydrochloride.
905:
meet the requirements for Content Uniformity with respect to propoxyphene hydrochloride.
Assay—
Mobile phase—
Mix 0.15% diethylamine in water, adjusted with phosphoric acid to a pH of 3.2 ± 0.2, and acetonitrile (4:1). Sonicate for 15 minutes, and filter through a filter having a porosity of 0.5 µm or finer. Make adjustments if necessary (see System Suitability under Chromatography 621).
621).
Standard preparation 1—
Transfer about 2J mg of USP Acetaminophen RS, accurately weighed, to a 10-mL volumetric flask, J being the ratio of the labeled amount, in mg, of acetaminophen to the labeled amount, in mg, of propoxyphene hydrochloride in each Tablet. Transfer about 2 mg of USP Propoxyphene Hydrochloride RS, accurately weighed, to the same flask. Add about 5 mL of Mobile phase, swirl to dissolve, dilute with Mobile phase to volume, and mix. This solution contains about 0.2 mg of USP Propoxyphene Hydrochloride RS and 0.2J mg of USP Acetaminophen RS per mL.
Standard preparation 2—
Transfer 5.0 mL of Standard preparation 1 to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix. This solution contains about 0.01J mg of USP Acetaminophen RS per mL.
Assay preparation 1—
Weigh and finely powder not less than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to about 40 mg of propoxyphene hydrochloride, to a 200-mL volumetric flask, add about 150 mL of Mobile phase, shake by mechanical means for 30 minutes, sonicate for 5 minutes, dilute with Mobile phase to volume, mix, and filter, discarding the first 20 mL of the filtrate. Use the clear filtrate as Assay preparation 1.
Assay preparation 2—
Transfer 5.0 mL of Assay preparation 1 to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Chromatographic system
(see Chromatography 621)—The liquid chromatograph is equipped with a 210-nm detector and a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph Standard preparation 1, and record the responses as directed for Procedure: the tailing factor for the propoxyphene peak is not more than 2.0, and the relative standard deviation for replicate injections is not more than 2.0%. Chromatograph Standard preparation 2, and record the responses as directed for Procedure: the tailing factor for the acetaminophen peak is not more than 1.5, and the relative standard deviation for replicate injections is not more than 2.0%.
621)—The liquid chromatograph is equipped with a 210-nm detector and a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph Standard preparation 1, and record the responses as directed for Procedure: the tailing factor for the propoxyphene peak is not more than 2.0, and the relative standard deviation for replicate injections is not more than 2.0%. Chromatograph Standard preparation 2, and record the responses as directed for Procedure: the tailing factor for the acetaminophen peak is not more than 1.5, and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure—
[note—Use peak areas where peak responses are indicated.] Separately inject equal volumes (about 20 µL) of Standard preparation 1, Standard preparation 2, Assay preparation 1, and Assay preparation 2 into the chromatograph, record the chromatograms using both the 210-nm and the 254-nm detectors, and measure the responses for the propoxyphene hydrochloride peaks obtained using the 210-nm detector and for the acetaminophen peaks obtained using the 254-nm detector. Calculate the quantity, in mg, of propoxyphene hydrochloride (C22H29NO2·HCl) in the portion of Tablets taken by the formula:
200C(rU / rS)
in which C is the concentration, in µg per mL, of USP Propoxyphene Hydrochloride RS in Standard preparation 1, and rU and rS are the propoxyphene hydrochloride peak responses obtained from Assay preparation 1 and Standard preparation 1, respectively. Calculate the quantity, in mg, of acetaminophen (C8H9NO2) in the portion of Tablets taken by the formula:
4000C(rU / rS)
in which C is the concentration, in mg per mL, of USP Acetaminophen RS in Standard preparation 2, and rU and rS are the acetaminophen peak responses obtained from Assay preparation 2 and Standard preparation 2, respectively.
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
Chromatographic Column—
| Topic/Question | Contact | Expert Committee |
| Monograph | Clydewyn M. Anthony, Ph.D.
Scientist 1-301-816-8139 |
(MDCCA05) Monograph Development-Cough Cold and Analgesics |
| Reference Standards | Lili Wang, Technical Services Scientist 1-301-816-8129 RSTech@usp.org |
|
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientist 1-301-816-8106 |
(BPC05) Biopharmaceutics05 |
USP32–NF27 Page 3419
Pharmacopeial Forum: Volume No. 30(1) Page 170
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.