Phenylalanine
» Phenylalanine contains not less than 98.5 percent and not more than 101.5 percent of C9H11NO2, as l-phenylalanine, calculated on the dried basis.
Packaging and storage
Preserve in well-closed containers.
Identification,
Infrared Absorption 197K.
Specific rotation 781S:
between 32.7 and 34.7.
Test solution:
20 mg per mL, in water.
pH 791:
between 5.4 and 6.0, in a solution (1 in 100).
Loss on drying 731
Dry it at 105 for 3 hours: it loses not more than 0.3% of its weight.
Residue on ignition 281:
not more than 0.4%.
Chloride 221
A 0.73-g portion shows no more chloride than corresponds to 0.50 mL of 0.020 N hydrochloric acid (0.05%).
Sulfate 221
A 0.33-g portion shows no more sulfate than corresponds to 0.10 mL of 0.020 N sulfuric acid (0.03%).
Iron 241:
0.003%.
Heavy metals, Method II 231:
0.0015%.
Chromatographic purity
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture.
Diluent
Prepare a mixture of glacial acetic acid and water (50:50).
Test solution
Dissolve an accurately weighed quantity of Phenylalanine in Diluent to obtain a solution having a concentration of 10 mg per mL. Apply 5 µL.
Standard solution
Dissolve an accurately weighed quantity of USP l-Phenylalanine RS in Diluent to obtain a solution having a known concentration of about 0.05 mg per mL. Apply 5 µL. [noteThis solution has a concentration equivalent to about 0.5% of that of the Test solution.]
System suitability solution
Prepare a solution in Diluent containing 0.4 mg each of USP l-Phenylalanine RS and USP l-Tyrosine RS per mL. Apply 5 µL.
Spray reagent
Dissolve 0.2 g of ninhydrin in 100 mL of a mixture of butyl alcohol and 2 N acetic acid (95:5).
Developing solvent system
Prepare a mixture of butyl alcohol, glacial acetic acid, and water (60:20:20).
Procedure
Proceed as directed for Thin-Layer Chromatography under Chromatography 621. After air-drying the plate, spray with Spray reagent, and heat between 100 and 105 for about 15 minutes. Examine the plate under white light. The chromatogram obtained from the System suitability solution exhibits two clearly separated spots. Any secondary spot in the chromatogram obtained from the Test solution is not larger or more intense than the principal spot in the chromatogram obtained from the Standard solution: not more than 0.5% of any individual impurity is found; and not more than 2.0% of total impurities is found.
Assay
Transfer about 160 mg of Phenylalanine, accurately weighed, to a 125-mL flask, dissolve in a mixture of 3 mL of formic acid and 50 mL of glacial acetic acid, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 16.52 mg of C9H11NO2.
Auxiliary Information
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Chromatographic Column
USP32NF27 Page 3280
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
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