Dihydroxyacetone
;)
1,3-Dihydroxy-2-propanone. [96-26-4].
»Dihydroxyacetone contains not less than 98.0percent and not more than 102.0percent of C3H6O3,calculated on the anhydrous basis.
Packaging and storage—
Preserve in tight containers in a cool place.
Identification—
A:
Infrared Absorption á197Kñ.
B:
The RFvalue of the principal spot in the chromatogram of the Test solutioncorresponds to that of the Standard preparationas obtained in the Chromatographic puritytest.
pHá791ñ:
between 4.0and 6.0,in a solution (1in 20).
Water,Method Iá921ñ:
not more than 0.2%.
Residue on ignition á281ñ:
not more than 0.1%.
Heavy metals,Method Iá231ñ:
0.001%.
Limit of iron á241ñ:
not more than 0.002%.
Chromatographic purity—
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture.
Glycerin solution—
Dilute an accurately measured volume of glycerin with methanol to obtain a solution having a concentration of about 0.25mg per mL.
Test solution—
Dissolve an accurately weighed quantity of Dihydroxyacetone in methanol to obtain a solution containing about 50mg per mL.
Standard solution—
Dissolve an accurately weighed quantity of USP Dihydroxyacetone RSin methanol,and mix to obtain a solution having a known concentration of about 50mg per mL.
Application volume:
1µL.
Developing solvent system:
a mixture of acetone and water (19:1).
Procedure—
Proceed as directed for Thin-Layer Chromatographyunder Chromatography á621ñ.Spray the plate with a mixture of toluene,a saturated solution of lead tetraacetate in glacial acetic acid,and a 1%solution of dichlorofluorescein in alcohol (190:5:1),and dry the plate for 5minutes at 105
.Examine the plate under short-wavelength UVlight,and compare the intensities of the glycerin spot observed in the chromatogram of the Test solutionwith that of the principal spot in the chromatogram of the Glycerin solution:the glycerin spot from the chromatogram of the Test solutionis not larger or more intense than the principal spot obtained from the Glycerin solution(0.5%),and no other secondary spots are observed in the chromatogram of the Test solution.
.Examine the plate under short-wavelength UVlight,and compare the intensities of the glycerin spot observed in the chromatogram of the Test solutionwith that of the principal spot in the chromatogram of the Glycerin solution:the glycerin spot from the chromatogram of the Test solutionis not larger or more intense than the principal spot obtained from the Glycerin solution(0.5%),and no other secondary spots are observed in the chromatogram of the Test solution.
Limit of protein—
Dissolve 25g of Dihydroxyacetone in 100mLof water.Transfer 100µLof this solution to a 5-mLvolumetric flask,dilute with brilliant blue G TSto volume,and mix.Determine the absorbance of this solution at about 595nm with a suitable spectrophotometer,using 100µLof water and 5mLof brilliant blue G TSas the blank:the absorbance of the test solution is not more than 0.400.
Assay—
Dissolve an accurately weighed quantity of about 0.1g of Dihydroxyacetone in 20mLof water,add 20mLof 0.1Mperiodic acid,and allow to stand at room temperature in the dark for 20minutes.Add about 3g of sodium bicarbonate,20mLof 0.6Mpotassium iodide,and 3mLof starch TS,and titrate with 0.05Msodium arsenite VS.Perform a blank titration,and make any necessary correction.Each mLof 0.05Msodium arsenite is equivalent to 4.504mg of C3H6O3.
Auxiliary Information—
Staff Liaison:Lawrence Evans,III,Ph.D.,Scientist
Expert Committee:(PA6)Pharmaceutical Analysis 6
USP28–NF23Page 652
Phone Number:1-301-816-8389