Pentazocine and Naloxone Tablets
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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
Pentazocine and Naloxone Tablets contain amounts of Pentazocine Hydrochloride and Naloxone Hydrochloride equivalent to NLT 90.0% and NMT 110.0% of the labeled amounts of pentazocine (C19H27NO) and naloxone (C19H21NO4).
2 IDENTIFICATION
A.
Diluent: Chloroform and methanol (1:1)
Standard solution A: 5.0 mg/mL of USP Pentazocine RS in Diluent
Standard solution B: 1.3 mg/mL of USP Naloxone RS in Diluent
Sample solution A: Crush 1 Tablet in 10 mL of Diluent. Sonicate for about 2 min, and filter.
Sample solution B: Evaporate 5 mL of Sample solution A to dryness on a steam bath under a stream of nitrogen. Dissolve the residue in 0.2 mL of Diluent.
Chromatographic system
(See Chromatography 〈621〉, Thin-Layer Chromatography.)
Adsorbent: 0.25-mm layer of chromatographic silica gel mixture
Application volume: 10 µL, Standard solution A and Sample solution A; 5 µL, Standard solution B and Sample solution B Developing solvent system: 1-Butanol, water, and glacial acetic acid (70:20:10)
Spray reagent: Folin-Ciocalteu Phenol TS followed by sodium hydroxide solution (1 in 10)
Analysis: Develop the chromatograms in the Developing solvent system until the solvent has moved about three-fourths of the length of the plate. Remove the plate from the chamber, mark the solvent front, and dry under a current of warm air. Spray the plate with Spray reagent. Acceptance criteria: Sample solution AF and Sample solution B exhibit spots having the same R values and approximately the same sizes and shapes as their respective Standard solutions.
3 ASSAY
Procedure
Diluent: Methanol, water, and phosphoric acid (500:500:1)
Solution A: Prepare a filtered and degassed mixture by dissolving 675 mg of sodium 1-octanesulfonate and 426 mg of anhydrous dibasic sodium phosphate in 625 mL of water, and mix.
Mobile phase: Add 475 mL of methanol and 10 mL of phosphoric acid to Solution A.
Strong anion-exchange resin: Transfer 30 g of strong anion-exchange resin to a 250-mL beaker. Wash the resin with two 200-mL portions of water, decanting the water after each wash. Wash with two 200-mL portions of dilute glacial acetic acid (1 in 20), decanting the first wash, and filter with the aid of suction.
Standard stock solution: 0.2 mg/mL of USP Naloxone RS in Diluent
Standard solution: Transfer 100 mg of USP Pentazocine RS to a 50-mL volumetric flask. Dissolve in about 30 mL of Diluent. Add 5.0 mL of the Standard stock solution, and dilute with Diluent to volume.
Sample solution: Transfer an amount nominally equivalent to 100 mg of pentazocine from NLT 20 Tablets to a 100-mL volumetric flask, and add 50.0 mL of Diluent. Sonicate for 5 min, and shake intermittently for 15 min. Filter into a glass-stoppered conical flask. Add about 250 mg of Strong anion-exchange resin, and shake for 30 min.
3.1 Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 229 nm
Column: 4.6-mm × 25-cm; packing L1
Flow rate: 1.5 mL/min
Injection volume: 20 µL
3.2 System suitability
Sample: Standard solution
[Note—The relative retention times for naloxone and pentazocine are about 0.3 and 1.0, respectively.]
Suitability requirements
Resolution: NLT 6 between pentazocine and naloxone
Relative standard deviation: NMT 2.0%
3.3 Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of pentazocine (C19H27NO) and naloxone (C19H21NO4) in the portion of Tablets taken:
Result = (rU /rS ) × (CS /CU ) × 100
rU = peak response of pentazocine or naloxone from the Sample solution
rS = peak response of pentazocine or naloxone from the Standard solution
CS = concentration of the appropriate USP Pentazocine RS or USP Naloxone RS in the Standard solution (mg/mL)
CU = nominal concentration of pentazocine or naloxone in the Sample solution (mg/mL)
Acceptance criteria: 90.0%–110.0% of the labeled amounts of pentazocine (C19H27NO) and naloxone (C19H21NO4)
4 PERFORMANCE TESTS
4.1 Dissolution 〈711〉
Medium: Water; 900 mL
Apparatus 2: 50 rpm
Time: 45 min
Detector: UV 279 nm (corrected for absorbance at 305 nm)
Standard solution: Dissolve a suitable amount of USP Pentazocine RS in a minimum volume of 0.1 N hydrochloric acid (about 25 mg/mL), diluting quantitatively and stepwise with water.
Sample solution: Filter portions of the solution under test, suitably diluted with Medium, if necessary.
Analysis: Determine the labeled amount of pentazocine (C19H27NO) dissolved in the Sample solution in comparison with the Standard solution.
Tolerances: NLT 75% (Q) of the labeled amount of pentazocine (C19H27NO) is dissolved.
Change to read:
4.2 Uniformity of Dosage Units 〈905〉: Meet the requirements (CN 1-Aug-2023)
Procedure for content uniformity
Diluent: Methanol, water, and phosphoric acid (500:500:1)
Solution A: Prepare a filtered and degassed mixture by dissolving 675 mg of sodium 1-octanesulfonate and 426 mg of anhydrous dibasic sodium phosphate in 625 mL of water, and mix.
Mobile phase: Add 475 mL of methanol and 10 mL of phosphoric acid to Solution A.
Strong anion-exchange resin: Transfer 30 g of strong anion-exchange resin to a 250-mL beaker. Wash the resin with two 200-mL portions of water, decanting the water after each wash. Wash with two 200-mL portions of dilute glacial acetic acid (1 in 20), decanting the first wash, and filter with the aid of suction.
Standard stock solution: 0.2 mg/mL of USP Naloxone RS in Diluent
Standard solution: Transfer 100 mg of USP Pentazocine RS to a 50-mL volumetric flask. Dissolve in about 30 mL of Diluent. Add 5.0 mL of the Standard stock solution, and dilute with Diluent to volume.
Sample solution: Transfer 1 Tablet to a 25-mL glass-stoppered cylinder. Add 25.0 mL of Diluent. Sonicate for 10 min, and shake intermittently for 15 min. Filter into a glass-stoppered conical flask. Add about 125 mg of Strong anion-exchange resin, and shake for 30 min.
4.2.1 Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 229 nm
Column: 4.6-mm × 25-cm; packing L1
Flow rate: 1.5 mL/min
Injection volume: 20 µL
4.2.2 System suitability
Sample: Standard solution [Note—The relative retention times for naloxone and pentazocine are about 0.3 and 1.0, respectively.] Suitability requirements
Resolution: NLT 6 between pentazocine and naloxone
Relative standard deviation: NMT 2.0%
4.2.3 Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of pentazocine (C19H27NO) and naloxone (C19H21NO4) in the portion of Tablets taken:
Result = (rU /rS) × (C /CU ) × 100
rU = peak response of pentazocine or naloxone from the Sample solution
rS = peak response of pentazocine or naloxone from the Standard solution
CS = concentration of the appropriate USP Pentazocine RS or USP Naloxone RS in the Standard solution (mg/mL)
CU = nominal concentration of pentazocine or naloxone in the Sample solution (mg/mL)
(CN 1-Aug-2023)
5 ADDITIONAL REQUIREMENTS
Packaging and Storage: Preserve in tight, light-resistant containers.
USP Reference Standards 〈11〉
USP Naloxone RS
USP Pentazocine RS
