SILDENAFIL CITRATE ORAL SUSPENSION标准

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PF 37(1) In-Process Revision: Sildenafil Citrate Oral Suspension

BRIEFING
Sildenafil Citrate Oral Suspension. Because there is no existing USP monograph for this dosage form, a new monograph is proposed. The liquid chromatographic procedure in the Assay is based on analyses performed with a 3.0-mm × 15-cm column that contains 5-µm packing L1. USP has received data indicating that a Zorbax C18 column is suitable. The typical retention time for sildenafil citrate is about 7.1 min.
(CMP: R. Schnatz.)
Correspondence Number—C86200
Comment deadline: March 31, 2011
Add the following:
Sildenafil Citrate Oral Suspension
DEFINITION

Sildenafil Citrate Oral Suspension contains NLT 90.0% and NMT 110.0% of the labeled amount of sildenafil citrate (C22H30N6O4S·C6H8O7).
Prepare Sildenafil Citrate Oral Suspension 2.5 mg/mL as follows (see Pharmaceutical Compounding—Nonsterile Preparations 795):
Sildenafil Citrate 250 mg
Vehicle: a mixture of Vehicle for Oral Solution, NF, and Vehicle for Oral Suspension, NF (1:1), a sufficient quantity to make 100 mL


Calculate the required quantity of each ingredient for the total amount to be prepared. If using tablets, place the required number in a suitable mortar, and comminute to a fine powder with a pestle or use Sildenafil Citrate powder. Add the Vehicle in small portions and triturate to make a smooth paste. Add increasing volumes of the Vehicle to make a sildenafil citrate liquid that is pourable. Transfer the contents of the mortar, stepwise and quantitatively, to a calibrated bottle. Add enough of the Vehicle to bring to final volume, and mix well.
ASSAY
•  Procedure
Mobile phase:  Prepare a solution of 0.2 M ammonium acetate and acetonitrile (50:50). Pass through a nylon 66 filter of 0.45-µm pore size, and degas with helium.
Standard stock solution:  1.0 mg/mL of sildenafil citrate in methanol. [Note—The Standard solutions should be prepared from the appropriate reference material. ]
Standard solution:  Pipet 1.0 mL of the Standard stock solution into a 10-mL volumetric flask, dilute with Mobile phase to volume to obtain a solution having a nominal concentration of 0.1 mg/mL of sildenafil citrate, and centrifuge.
Sample solution:  Shake thoroughly by hand each bottle of Oral Suspension. Pipet 4.0 mL of Oral Suspension to a 10-mL volumetric flask, and dilute with methanol to volume. Pipet 1.0 mL of the diluted solution to a 10-mL volumetric flask, further dilute with Mobile phase to volume to obtain a solution with a nominal concentration of 0.1 mg/mL of sildenafil citrate, and centrifuge.
Chromatographic system  
(See Chromatography 621, System Suitability.)
Mode:  LC
Detector:  UV 245 nm
Column:  3.0-mm × 15-cm; 5-µm packing L1
Column temperature:  25
Flow rate:  0.5 mL/min
Injection size:  10 µL
System suitability  
Sample:  Standard solution
[NOTE—The retention time for sildenafil citrate is about 7.1 min.]
Suitability requirements  
Relative standard deviation:  NMT 2.0% for replicate injections
Analysis  
Samples:  Standard solution and Sample solution

Calculate the percentage of the labeled amount of sildenafil citrate (C22H30N6O4S·C6H8O7) in the portion of Oral Suspension taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response of the Sample solution
rS = peak response of the Standard solution
CS = concentration of sildenafil citrate in the Standard solution (µg/mL)
CU = nominal concentration of sildenafil citrate in the Sample solution (µg/mL)

Acceptance criteria:  90.0%–110.0%
SPECIFIC TESTS
•  pH 791: 3.9–4.9
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Package in tight, light-resistant containers. Store at controlled cold temperature or at controlled room temperature.
•  Labeling: Label it to indicate that it is to be well-shaken before use, and to state the Beyond-Use Date.
•  Beyond-Use Date: NMT 90 days after the date on which it was compounded, when stored at controlled cold temperature or controlled room temperatureUSP35
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