Primaquine Phosphate Tablets
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.USP35
Mobile phase:
Acetonitrile, tetrahydrofuran, trifluoroacetic acid, and water (9: 1: 0.1: 90)
905
:
Meet the requirements
• Organic Impurities
USP35
11
USP35
DEFINITION
Primaquine Phosphate Tablets contain NLT 93.0% and NMT 107.0% of the labeled amount of primaquine phosphate (C15H21N3O·2H3PO4).
IDENTIFICATION
• A.
Sample solution:
Digest the equivalent to 25 mg of primaquine phosphate from a quantity of finely powdered Tablets with 10 mL of water for 15 min, and filter.
Analysis:
Dilute 0.1 mL of the Sample solution with 1 mL of water, and add 1 drop of gold chloride TS.
Acceptance criteria:
A violet-blue color is produced at once.
Change to read:
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.USP35
ASSAY
Change to read:
• Procedure
Mobile phase:
Acetonitrile, tetrahydrofuran, trifluoroacetic acid, and water (9: 1: 0.1: 90)
Standard solution:
0.4 mg/mL of USP Primaquine Phosphate RS in Mobile phase. [Note—Sonicate with intermittent shaking to dissolve, if necessary. ]
System suitability stock solution:
0.4 mg/mL of USP Primaquine Related Compound A RS in Mobile phase
System suitability solution:
Transfer 1.0 mL of System suitability stock solution to a 10-mL volumetric flask, and dilute with Standard solution to volume.
Sensitivity solution:
0.2 µg/mL of USP Primaquine Phosphate RS from Standard solution
Sample stock solution:
Transfer a quantity of Tablets (NLT 20), accurately counted and weighed, to a 500-mL volumetric flask. Add 300 mL of Mobile phase, then sonicate and shake for 15 min. Add 150 mL of Mobile phase, then sonicate and shake for 15 min. Dilute with Mobile phase to volume, and filter.
Sample solution:
0.4 mg/mL of primaquine phosphate in Mobile phase from the Sample stock solution
Chromatographic system
Mode:
LC
Detector:
UV 265 nm
Column:
4.6-mm × 75-mm; 3-µm packing L7
Flow rate:
1.5 mL/min
Injection size:
10 µL
Run time:
Three times the retention time of primaquine
System suitability
Samples:
Standard solution, System suitability solution, and Sensitivity solution
Suitability requirements
Resolution:
NLT 2.5 between primaquine phosphate and primaquine related compound A, System suitability solution
Relative standard deviation:
NMT 1.0% for primaquine phosphate, Standard solution
Signal-to-noise ratio:
NLT 10 for the primaquine peak, Sensitivity solution
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of primaquine phosphate (C15H21N3O·2H3PO4) in the portion of Tablets 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 Primaquine Phosphate RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of primaquine phosphate in the Sample solution (mg/mL) |
Acceptance criteria:
93.0%–107.0%USP35
USP35
PERFORMANCE TESTS
• Dissolution 711
711
Medium:
0.01 N hydrochloric acid; 900 mL
Apparatus 2:
50 rpm
Time:
60 min
Sample solution:
Pass a portion of the solution under test through an appropriate filter.
Standard solution:
USP Primaquine Phosphate RS in Medium in a concentration similar that of the Sample solution
Solution A:
961 mg of sodium 1-pentanesulfonate and 1 mL of glacial acetic acid in 400 mL of water
Mobile phase:
Methanol and Solution A (3:2)
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
3.9-mm × 30-cm; packing L1
Flow rate:
2 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Relative standard deviation:
NMT 3.0%
Analysis
Samples:
Sample solution and Standard solution
Calculate the amount of primaquine phosphate (C15H21N3O·2H3PO4) dissolved.
Tolerances:
NLT 80% (Q) of the labeled amount of primaquine phosphate (C15H21N3O·2H3PO4) is dissolved.
Change to read:
• Uniformity of Dosage Units 905:
Meet the requirements
Procedure for content uniformity:
Transfer 1 Tablet to a 50-mL volumetric flask, add about 30 mL of Mobile phase, then sonicate and shake for 15 min. Add Mobile phase up to the neck of the flask, then sonicate and shake for additional 15 min. Allow the solution to cool, and dilute with Mobile phase to volume. Filter a portion of the solution, and dilute 8.0 mL of this filtered solution with Mobile phase to 10.0 mL. Analyze the solution as directed in the Assay.USP35
Transfer 1 Tablet to a 50-mL volumetric flask, add about 30 mL of Mobile phase, then sonicate and shake for 15 min. Add Mobile phase up to the neck of the flask, then sonicate and shake for additional 15 min. Allow the solution to cool, and dilute with Mobile phase to volume. Filter a portion of the solution, and dilute 8.0 mL of this filtered solution with Mobile phase to 10.0 mL. Analyze the solution as directed in the Assay.USP35
IMPURITIES
Add the following:
• Organic Impurities
Mobile phase, Standard solution, System suitability solution, Sensitivity solution, Sample solution, Chromatographic system, and System suitability:
Proceed as directed in the Assay.
Analysis
Sample:
Sample solution
Calculate the percentage of each impurity in the portion of Tablets taken:
Result = (rU/rT) × 100
| rU | = | = peak response of each impurity from the Sample solution |
| rT | = | = peak response of primaquine phosphate from the Sample solution |
Acceptance criteria:
See Table 1.
[Note—Disregard any impurity less than 0.05%. ]
Table 1
| Name | Relative Retention Time |
Acceptance Criteria, NMT (%) |
|---|---|---|
| Specified unidentified impuritya | 0.24 | — |
| Specified unidentified impurity | 0.29 | 0.60 |
| Primaquine related compound Aa,b | 0.80 | — |
| Primaquine | 1.0 | — |
| Specified unidentified impuritya | 1.8 | — |
| Any other individual impurity | — | 0.20 |
| Total impurities | — | 1.0 |
|
a
These process impurities are listed for information only and are not quantified in the drug product.
b
8-[(4-Aminopentyl)amino]-6-methoxyquinoline.
|
||
USP35ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed, light-resistant containers.
Change to read:
• USP Reference Standards 11
USP Primaquine Phosphate RS 
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USP Primaquine Related Compound A RS
8-[(4-Aminopentyl)amino]-6-methoxyquinoline.
C15H21N3O 259.35
8-[(4-Aminopentyl)amino]-6-methoxyquinoline.
C15H21N3O 259.35
USP35
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Leonel M. Santos, Ph.D.
Senior Scientific Liaison 1-301-816-8168 |
(SM12010) Monographs - Small Molecules 1 |
| 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 4412
Pharmacopeial Forum: Volume No. 37(1)