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Dexchlorpheniramine Maleate
L51 | Amylose tris-3,5-dimethylphenylcarbamate-coated, porous, spherical, silica partilces, 5 to 10 µm in diameter. | Chiralpak AD |
Dexchlorpheniramine Maleate
(dex'' klor fen ir' a meen mal' ee ate).
DEFINITION
Dexchlorpheniramine Maleate, dried at 65 for 4 h, contains NLT 98.0% and NMT 102.0% of dexchlorpheniramine maleate (C16H19ClN2·C4H4O4).
IDENTIFICATION
• B. The retention times of the maleic acid and dexchlorpheniramine peaks of the Sample solution correspond to those of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Solution A: 5.44 g/L of monobasic potassium phosphate. Adjust with phosphoric acid to a pH of 3.0 ± 0.1.
Solution B: Acetonitrile
Diluent: Acetonitrile and Solution A (5:95)
System suitability stock solution: 0.02 mg/mL each of USP Pheniramine Maleate RS, USP Chlorpheniramine Related Compound B RS, and USP Chlorpheniramine Related Compound C RS in Diluent. Sonicate for 1 min.
System suitability solution: 0.5 mg/mL of USP Dexchlorpheniramine Maleate RS and 2 µg/mL each of USP Pheniramine Maleate RS, USP Chlorpheniramine Related Compound B RS, and USP Chlorpheniramine Related Compound C RS in Diluent, prepared as follows. Transfer 5.0 mg of USP Dexchlorpheniramine Maleate RS to a 10-mL volumetric flask, add 5 mL of Diluent and 1.0 mL of the System suitability stock solution, and dilute with Diluent to volume. Sonicate for 1 min.
Standard solution: 0.5 mg/mL of USP Dexchlorpheniramine Maleate RS in Diluent. Sonicate for 1 min.
Sample solution: 0.5 mg/mL of Dexchlorpheniramine Maleate in Diluent. Sonicate for 1 min.
Chromatographic system
Mode: LC
Detector: UV 225 nm
Column: 4.6-mm × 25-cm; 5-µm packing L1
Column temperature: 30
Flow rate: 1 mL/min
Injection volume: 10 µL
System suitability
Samples: System suitability solution and Standard solution
[NOTE—The relative retention times of maleic acid, chlorpheniramine related compound C, and dexchlorpheniramine are 0.18, 0.94, and 1.0, respectively. ]
Suitability requirements
Resolution: NLT 1.5 between chlorpheniramine related compound C and dexchlorpheniramine; NLT 2.0 between chlorpheniramine related compound B and pheniramine, System suitability solution
Tailing factor: NMT 2.0, Standard solution
Relative standard deviation: NMT 0.73%, Standard solution
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of dexchlorpheniramine maleate (C16H19ClN2·C4H4O4) in the portion of Dexchlorpheniramine Maleate taken:
Result = (rU/rS) × (CS/CU) × 100
rU | = | = peak response fordexchlorpheniramine from the Sample solution |
rS | = | = peak response fordexchlorpheniramine from theStandard solution |
CS | = | = concentration of USPDexchlorpheniramine Maleate RS in the Standard solution (mg/mL) |
CU | = | = concentration of DexchlorpheniramineMaleate in the Sample solution(mg/mL) |
Acceptance criteria: 98.0%–102.0%, previously dried at 65 for 4 h
IMPURITIES
• Residue on Ignition 281: NMT 0.2%
Change to read:
• Organic ImpuritiesSolution A, Solution B, Diluent, System suitability solution, Mobile phase, and Chromatographic system: Proceed as directed in the Assay.
Standard solution: 2.8 µg/mL of USP Dexchlorpheniramine Maleate RS in Diluent,(ERR 1-Oct-2014) equivalent to 2.0 µg/mL of dexchlorpheniramine. Sonicate for 1 min.
Sensitivity solution: 0.74 µg/mL of USP Pheniramine Maleate RS in Diluent
Sample solution: 0.5 mg/mL of Dexchlorpheniramine Maleate in Diluent. Sonicate for 1 min.
System suitability
Samples: System suitability solution, Standard solution, and Sensitivity solution
Suitability requirements
Resolution: NLT 1.5 between chlorpheniramine related compound C and dexchlorpheniramine; NLT 2.0 between chlorpheniramine related compound B and pheniramine, System suitability solution
Signal-to-noise ratio: NLT 10, Sensitivity solution
Relative standard deviation: NMT 5.0%, Standard solution
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Dexchlorpheniramine Maleate taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
rU | = | = peak response of each impurity from theSample solution |
rS | = | = peak response ofdexchlorpheniramine from theStandard solution |
CS | = | = concentration of dexchlorpheniraminein the Standard solution (mg/mL) |
CU | = | = concentration of DexchlorpheniramineMaleate in the Sample solution(mg/mL) |
F | = | = relative response factor (see Table 2) |
Acceptance criteria: See Table 2. Disregard peaks having areas less than 0.05% of dexchlorpheniramine.
Table 2
Name | Relative Retention Time | Relative Response Factor | Acceptance Criteria, NMT (%) |
---|---|---|---|
Maleic acida | 0.18 | — | — |
Chlorpheniramine related compound Bb | 0.49 | — | — |
Pheniramine | 0.57 | 0.40 | 0.4 |
Chlorpheniramine related compound Cc | 0.97 | — | — |
Dexchlorpheniramine | 1.0 | — | — |
Any other unspecified impurity | — | 1.0 | 0.10 |
Total impurities | — | — | 1 |
a Salt counter ion is included in the table for identification purposes only. b Di(pyridin-2-yl)amine. Used only to establish system suitability. c 3-(4-Chlorophenyl-N-methyl-3-(pyridin-2-yl)propan-1-amine. Used only to establish system suitability. |
• Enantiomeric Purity
System suitability solution: 0.7 mg/mL of chlorpheniramine in 2-propanol prepared as follows. Dissolve 10.0 mg of USP Chlorpheniramine Maleate RS in 3 mL of water. Make the solution basic by adding a few drops of concentrated ammonium hydroxide, and shake with 5 mL of methylene chloride. Separate the layers and evaporate the lower, methylene chloride layer on a water bath until an oily residue is obtained. Dissolve the residue, and dilute with 2-propanol to 10.0 mL.
Standard stock solution: 0.7 mg/mL of dexchlorpheniramine in 2-propanol prepared as follows. Dissolve 10.0 mg of USP Dexchlorpheniramine Maleate RS in 3 mL of water. Make the solution basic by adding a few drops of concentrated ammonium hydroxide, and shake with 5 mL of methylene chloride. Separate the layers and evaporate the lower, methylene chloride layer on a water bath until an oily residue is obtained. Dissolve the residue, and dilute with 2-propanol to 10.0 mL.
Standard solution: 0.014 mg/mL of dexchlorpheniramine in 2-propanol from the Standard stock solution
Sample solution: 0.7 mg/mL of dexchlorpheniramine in 2-propanol prepared as follows. Dissolve 10.0 mg of Dexchlorpheniramine Maleate in 3 mL of water. Make the solution basic by adding a few drops of concentrated ammonium hydroxide, and shake with 5 mL of methylene chloride. Separate the layers and evaporate the lower, methylene chloride layer on a water bath until an oily residue is obtained. Dissolve the residue, and dilute with 2-propanol to 10.0 mL.
Mobile phase: n-Hexane, 2-propanol, and diethylamine (980:20:3)
Chromatographic system
Mode: LC
Detector: UV 254 nm
Column: 4.6-mm × 25-cm; 10-µm packing L51
Flow rate: 1 mL/min
Injection volume: 10 µL
System suitability
[NOTE—Under these conditions the dexchlorpheniramine (S-enantiomer) elutes first. ]
Sample: System suitability solution
Suitability requirements
Resolution: NLT 1.5 between the R-enantiomer and dexchlorpheniramine (S-enantiomer)
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the R-enantiomer in the portion of dexchlorpheniramine taken:
Result = (rU/rS) × (CS/CU) × 100
rU | = | = peak response of the R-enantiomer from the Sample solution |
rS | = | = peak response ofdexchlorpheniramine from theStandard solution |
CS | = | = concentration of dexchlorpheniraminein the Standard solution (mg/mL) |
CU | = | = concentration of dexchlorpheniraminein the Sample solution (mg/mL) |
Acceptance criteria: NMT 2%
SPECIFIC TESTS
• Optical Rotation, Specific Rotation781S
Sample solution: 50 mg/mL, in dimethylformamide
Acceptance criteria: +39.5 to +43.0
ADDITIONAL REQUIREMENTS
• Packaging and Storage: Preserve in tight, light-resistant containers.
• USP Reference Standards 11
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question | Contact | Expert Committee |
---|---|---|
Monograph | Alan R Potts, PhD Principal Scientific Liaison (301) 816-8364 | (SM42010) Monographs - Small Molecules 4 |
Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP38–NF33 Page 3044
Pharmacopeial Forum: Volume No. 38(6)Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 38 or NF 33.
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