Flavoxate Hydrochloride
(flay vox' ate hye'' droe klor' ide).
C24H25NO4·HCl 427.92 4H-1-Benzopyran-8-carboxylic acid, 3-methyl-4-oxo-2-phenyl-, 2-(1-piperidinyl)ethyl ester, hydrochloride; 2-Piperidinoethyl 3-methyl-4-oxo-2-phenyl-4H-1-benzopyran-8-carboxylate hydrochloride [3717-88-2]. DEFINITION
Flavoxate Hydrochloride contains NLT 98.0% and NMT 102.0% of C24H25NO4·HCl, calculated on the dried basis.
IDENTIFICATION
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
• C. Identification TestsGeneral, Chloride 191:
A solution of 10 mg/mL meets the requirements of the silver nitrate precipitate.
ASSAY
• Procedure
Solution A:
Mixture of 1.0 g of sodium hexanesulfonate in 650 mL of water, 1 mL of triethylamine, and 1.0 mL of phosphoric acid
Mobile phase:
Add 350 mL of acetonitrile to Solution A.
Standard solution:
50 µg/mL of USP Flavoxate Hydrochloride RS in Mobile phase
Sample solution:
50 µg/mL of Flavoxate Hydrochloride in Mobile phase
Chromatographic system
Mode:
LC
Detector:
UV 293 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Flow rate:
1 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
[NoteThe retention time of flavoxate is about 4.3 min. ]
Suitability requirements
Column efficiency:
NLT 3000 theoretical plates
Tailing factor:
NMT 2.0
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C24H25NO4·HCl in the portion of Flavoxate Hydrochloride taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
98.0%102.0% on the dried basis
IMPURITIES
Organic Impurities
• Procedure
Solution A:
0.05% (v/v) trifluoroacetic acid in water
Solution B:
Acetonitrile
Mobile phase:
See the gradient table below.
Diluent:
Methanol and 0.02% trifluoroacetic acid (1:1)
Standard stock solution 1:
2 mg/mL of USP Flavoxate Hydrochloride RS in Diluent
Standard stock solution 2:
0.05 mg/mL of USP Flavoxate Related Compound A RS in Diluent
Standard stock solution 3:
0.05 mg/mL of USP Flavoxate Related Compound B RS in methanol
Standard stock solution 4:
0.05 mg/mL of USP Flavoxate Related Compound C RS prepared as follows: Dissolve USP Flavoxate Related Compound C RS first in methanol using 10% of final volume, then fill 10% of final volume with 0.02% trifluoroacetic acid. Dilute with Diluent to volume.
Standard solution:
1 mg/mL of USP Flavoxate Hydrochloride RS and 5 µg/mL each of USP Flavoxate Related Compound A RS, USP Flavoxate Related Compound B RS, and USP Flavoxate Related Compound C RS in Diluent from Standard stock solutions 1, 2, 3, and 4, respectively
Sample solution:
1 mg/mL of Flavoxate Hydrochloride in Diluent
Chromatographic system
Mode:
LC
Detector:
UV 240 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Column temperature:
30
Flow rate:
0.8 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Resolution:
NLT 2.0 between the flavoxate related compound B and flavoxate related compound C peaks
Tailing factor:
NMT 1.5 for the flavoxate related compounds A, B, and C peaks
Relative standard deviation:
NMT 2.0% for the flavoxate peak
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of flavoxate related compounds A, B, and C in the portion of Flavoxate Hydrochloride taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
Calculate the percentage of any other unspecified degradation product in the portion of Flavoxate Hydrochloride taken:
Result = (rU/rT) × 100
Acceptance criteria
Individual impurities:
See Impurity Table 1.
Total impurities:
1.0%
Impurity Table 1
SPECIFIC TESTS
• Loss on Drying 731:
Dry a sample at 105 to constant weight: it loses NMT 0.5% of its weight.
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, protected from light; and store at room temperature.
• USP Reference Standards 11
USP Flavoxate Hydrochloride RS
USP Flavoxate Related Compound A RS
3-Methylflavone-8-carboxylic acid. C17H12O4 280.27
USP Flavoxate Related Compound B RS
3-Methylflavone-8-carboxylic acid methyl ester. C18H14O4 294.30
USP Flavoxate Related Compound C RS
3-Methylflavone-8-carboxylic acid ethyl ester. C19H16O4 308.33
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3198
Pharmacopeial Forum: Volume No. 35(6) Page 1454
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