Ropinirole Hydrochloride
C16H24N2O·HCl 296.84
2H-Indol-2-one, 4-[2-(dipropylamino)ethyl]-1,3-dihydro-, monohydrochloride;
4-[2-(Dipropylamino)ethyl]-2-indolinone monohydrochloride
[91374-20-8].
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C16H24N2O·HCl 296.84
2H-Indol-2-one, 4-[2-(dipropylamino)ethyl]-1,3-dihydro-, monohydrochloride;
4-[2-(Dipropylamino)ethyl]-2-indolinone monohydrochloride
[91374-20-8].DEFINITION
Ropinirole Hydrochloride contains NLT 98.0% and NMT 102.0% of C16H24N2O·HCl, calculated on the anhydrous basis.
IDENTIFICATION
• B.
The retention time of the ropinirole hydrochloride peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Buffer:
1.88 g of sodium 1-hexanesulfonate and 1 g of phosphoric acid in 1 L of water. Adjust with dilute triethylamine solution (1 mL/10 mL) to a pH of 6.5.
Diluent:
Acetonitrile and water (1:4)
Mobile phase:
Acetonitrile and Buffer (1:4)
Standard solution:
0.1 mg/mL of USP Ropinirole Hydrochloride RS in Diluent. Sonication may be used to aid dissolution.
Sample solution:
0.1 mg/mL of Ropinirole Hydrochloride in Diluent. Sonication may be used to aid dissolution.
Chromatographic system
Mode:
LC
Detector:
UV 215 nm
Column:
4.6-mm × 25-cm; 5-µm packing L7
Column temperature:
30
Flow rate:
1.0 mL/min
Injection size:
10 µL
Run time:
2.5 times the retention time of ropinirole
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 1.6
Relative standard deviation:
NMT 1.5%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C16H24N2O·HCl in the portion of Ropinirole Hydrochloride taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of the Standard solution (mg/mL) |
| CU | = | = concentration of the Sample solution (mg/mL) |
Acceptance criteria:
98.0%–102.0% on the anhydrous basis
IMPURITIES
SPECIFIC TESTS
• Water Determination, Method Ic 
921
:
NMT 0.5%
921:
NMT 0.5%
• Limit of Pd
[Note—Perform this test if Pd is a known inorganic impurity. ]
Solution A:
Dissolve 2.4 g of sodium hydroxide in 20 mL of water, and dilute with glycerol to 100 mL.
Solution B:
40 mg/mL of thioacetamide in water. [Note—Solution may be filtered if necessary. ]
Buffer:
Carefully add 27 mL of hydrochloric acid to 25 g of ammonium acetate, and dilute with water to 100 mL.
Pd standard solution:
10 ppm of Pd from commercially available ICP grade 1000 ppm Pd stock solution
Standard solution:
Pipet 1.0 mL of Pd standard solution into a platinum crucible, and gently evaporate to dryness. Moisten the residue with 0.5 mL of sulfuric acid, and heat with a bunsen burner until fumes are no longer emitted. Place the crucible in a muffle furnace at 700, and heat for 5 additional min. Cool, add 5 mL of hydrochloric acid to the residue, and evaporate to dryness. Add 1 mL of 2 M hydrochloric acid and, if necessary, dissolve the residue with gentle heating. When cool, transfer the contents to a 50-mL beaker. Wash the crucible twice with 1-mL aliquots of water, and add the washings to the beaker. Pass the solution through a 2-µm membrane filter into a centrifuge tube.
, and heat for 5 additional min. Cool, add 5 mL of hydrochloric acid to the residue, and evaporate to dryness. Add 1 mL of 2 M hydrochloric acid and, if necessary, dissolve the residue with gentle heating. When cool, transfer the contents to a 50-mL beaker. Wash the crucible twice with 1-mL aliquots of water, and add the washings to the beaker. Pass the solution through a 2-µm membrane filter into a centrifuge tube.
Sample solution:
Transfer 1 g of Ropinirole Hydrochloride to a platinum crucible, and heat over a bunsen burner until the material is completely carbonized. Moisten the contents with 0.5 mL of sulfuric acid, and heat over a bunsen burner until fumes are no longer emitted. Place the crucible in a muffle furnace at 700, and heat until all the organic material has been destroyed. When cool, add 5 mL of hydrochloric acid to the residue and evaporate to dryness. Add 1 mL of 2 M hydrochloric acid and, if necessary, dissolve the residue with gentle heating. When cool, transfer the contents to a 50-mL beaker. Wash the crucible twice with 1-mL aliquots of water, and add the washings to the beaker. Pass the solution through a 2-µm membrane filter into a centrifuge tube.
, and heat until all the organic material has been destroyed. When cool, add 5 mL of hydrochloric acid to the residue and evaporate to dryness. Add 1 mL of 2 M hydrochloric acid and, if necessary, dissolve the residue with gentle heating. When cool, transfer the contents to a 50-mL beaker. Wash the crucible twice with 1-mL aliquots of water, and add the washings to the beaker. Pass the solution through a 2-µm membrane filter into a centrifuge tube.
Analysis:
To the filtered Standard solution and Sample solution add 1 mL of Solution A, 0.2 mL of Solution B, and 2 mL of Buffer. Cap the centrifuge tubes securely, and incubate at 37 for 2 h. Pass the Sample solution and Standard solution through a 2-µm membrane filter, wash the membrane with 2-mL aliquots of water, and allow the membrane to dry.
for 2 h. Pass the Sample solution and Standard solution through a 2-µm membrane filter, wash the membrane with 2-mL aliquots of water, and allow the membrane to dry.
Acceptance criteria:
The intensity of the spot due to the sample is not more intense than the spot due to the standard (10 ppm).
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, and store at room temperature.
• USP Reference Standards 11
11
USP Ropinirole Hydrochloride RS 
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USP Ropinirole Related Compound A RS
4-(2-Hydroxyethyl)indolin-2-one.
C10H11NO2 177.20
4-(2-Hydroxyethyl)indolin-2-one.
C10H11NO2 177.20
USP Ropinirole Related Compound B RS
4-[2-(Dipropylamino)ethyl]indoline-2,3-dione.
C16H22N2O2 274.36
4-[2-(Dipropylamino)ethyl]indoline-2,3-dione.
C16H22N2O2 274.36
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Hariram Ramanathan, M.S.
Associate Scientific Liaison 1-301-816-8313 |
(SM42010) Monographs - Small Molecules 4 |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 4586
Pharmacopeial Forum: Volume No. 36(1) Page 133