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2-Naphthacenecarboxamide, 4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11dioxo-, monohydrochloride, [4S-(4,4a,5a,12a)]-;
4,7-Bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-naphthacenecarboxamide monohydrochloride [13614-98-7].
Minocycline Hydrochloride contains the equivalent of NLT 890 µg and NMT 950 µg of minocycline (C23H27N3O7) per mg, calculated on the anhydrous basis.
• Infrared Absorption 197K: Dry the Standard and Sample at 100 for 2 h before use.
[NoteProtect the Standard solution and Sample solution from light, store in a refrigerator, and use within 3 h. ]
Mobile phase: Dimethylformamide, tetrahydrofuran, 0.2 M ammonium oxalate, and 0.01 M edetate disodium (120:80:600:180). Adjust with ammonium hydroxide to a pH of 7.2.
System suitability solution: Dissolve 10 mg of USP Minocycline Hydrochloride RS in 20 mL of 0.2 M ammonium oxalate. Heat on a water bath at 60 for 3 h, allow to cool, and dilute with water to 25.0 mL.
Standard solution: Equivalent to 500 µg/mL of minocycline (C23H27N3O7) from USP Minocycline Hydrochloride RS in water
Sample solution: Equivalent to 500 µg/mL of minocycline (C23H27N3O7) from Minocycline Hydrochloride in water
Detector: UV 280 nm
Column: 4.6-mm × 25-cm; 5-µm packing L1
Column temperature: 40
Flow rate: 1.5 mL/min
Injection size: 20 µL
Samples: System suitability solution and Standard solution
[NoteThe relative retention times for epiminocycline and minocycline are 0.7 and 1.0, respectively. ]
Resolution: NLT 4.6 between epiminocycline and minocycline, System suitability solution
Tailing factor: 0.92.0 for the analyte peak, Standard solution
Relative standard deviation: NMT 2.0%, Standard solution
Samples: Standard solution and Sample solution
Calculate the quantity, in µg/mg, of minocycline (C23H27N3O7) in the portion of Minocycline Hydrochloride taken:
Result = (rU/rS) × (CS/CU) × P
Acceptance criteria: 890950 µg/mg on the anhydrous basis
Mobile phase and System suitability solution: Proceed as directed in the Assay
[NoteProtect the Sample solutions from light, store in a refrigerator, and use within 3 h. ]
Sample solution 1: 0.25 mg/mL of Minocycline Hydrochloride
Sample solution 2: 5 µg/mL of Minocycline Hydrochloride in water
Sample solution 3: 3 µg/mL of Minocycline Hydrochloride in water
Chromatographic system: Proceed as directed in the Assay.
Run time: 2.6 times the retention time of minocycline, Sample solution 1
Samples: Sample solution 1, Sample solution 2, and Sample solution 3
Calculate the percentage of epiminocycline in the portion of Minocycline Hydrochloride taken:
Result = (rE1/rM3) × D1 × 100
Calculate the total percentage of impurities other than epiminocycline in the portion of Minocycline Hydrochloride taken:
Result = (rT/rM2) × D2 × 100
Individual impurities: NMT 1.2% epiminocycline
Total impurities (excluding epiminocycline): NMT 2.0%
• Crystallinity 695: Meets the requirements
• pH 791: 3.54.5, in a solution equivalent to 10 mg/mL of minocycline
• Water Determination, Method I 921: 4.3%8.0%
• Sterility Tests 71: Where the label states that Minocycline Hydrochloride is sterile, it meets the requirements.
• Bacterial Endotoxins Test 85: Where the label states that Minocycline Hydrochloride is sterile or must be subjected to further processing during the preparation of injectable dosage forms, it contains NMT 1.25 USP Endotoxin Units/mg of minocycline.
• Packaging and Storage: Preserve in tight containers, protected from light.
• Labeling: Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
• USP Reference Standards 11
USP Endotoxin RS
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3926Pharmacopeial Forum: Volume No. 36(2) Page 418