Dimethyl Sulfoxide Topical Solution
» Dimethyl Sulfoxide Topical Solution contains not less than 90.0 percent and not more than 110.0 percent of the labeled concentration of C2H6OS.
Packaging and storage Preserve in tight, light-resistant containers.
Labeling Label it to indicate that it is for veterinary use only.
USP Reference standards 11
A: The chromatogram of the Assay preparation, obtained as directed in the Assay, exhibits a major peak for dimethyl sulfoxide, the retention time of which corresponds to that exhibited in the chromatogram of the Standard preparation, obtained as directed in the Assay.
B: To 2 mL of Topical Solution in a test tube add 5 mL of cold hydriodic acid. Filter the mixture rapidly, and collect the precipitate. Dry the precipitate in vacuum: a deep violet, crystalline solid is obtained, and it is soluble in chloroform, yielding a red solution.
C: To 0.1 g of solid sodium hydroxide in a test tube add 10 mL of Topical Solution, and heat on a steam bath until the sodium hydroxide has dissolved. Add 10 mL of chloroform, and shake. Filter the chloroform layer through a filter funnel containing about 10 g of anhydrous sodium sulfate. Heat the filtrate on a steam bath to remove the chloroform. Determine the IR spectrum of the liquid residue as directed under Spectrophotometric Identification Tests 197F. The spectrum so obtained corresponds to that of a spectrum of USP Dimethyl Sulfoxide RS, similarly prepared.
Assay [noteUse glass equipment to prepare solutions. ]
Internal standard solution Transfer 3.0 mL of dimethylformamide to a 250-mL volumetric flask. Add about 200 mL of acetone, and shake for about 1 minute. Dilute with acetone to volume, and mix.
Standard preparation Transfer about 2 g of USP Dimethyl Sulfoxide RS, accurately weighed, to a 250-mL volumetric flask, add 3.0 mL of dimethylformamide and 200 mL of acetone, and sonicate for about 1 minute. Dilute with acetone to volume, and mix to obtain a solution having a known concentration of about 8 mg of USP Dimethyl Sulfoxide RS per mL.
Assay preparation Transfer an accurately measured volume of Topical Solution, equivalent to about 2 g of dimethyl sulfoxide, to a 250-mL volumetric flask, add 3.0 mL of dimethylformamide and about 200 mL of acetone, and sonicate for about 1 minute. Dilute with acetone to volume, and mix.
Chromatographic system (see Chromatography 621)The gas chromatograph is equipped with a flame-ionization detector and a 4-mm × 1.8-m column packed with 10% liquid phase G16 on support S1A. The column is maintained at about 170, the injection port at about 200, and the detector block at about 300. The carrier gas is helium, flowing at a rate of about 20 mL per minute. Chromatograph two portions of the acetone used to prepare the Standard preparation, the Assay preparation, and the Internal standard solution, and record the peak responses as directed under Procedure. Discard the first chromatogram, and examine the second to confirm that there are no peaks present that would interfere with the measurement of the dimethylformamide peaks and the dimethyl sulfoxide peaks in subsequent chromatograms. Chromatograph the Internal standard solution, and record the peak responses as directed for Procedure: examine the chromatogram to confirm that there are no peaks present that would interfere with the measurement of the dimethylformamide peaks and the dimethyl sulfoxide peaks in subsequent chromatograms. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative retention times are about 0.2 for acetone, 0.5 for dimethylformamide, and 1.0 for dimethyl sulfoxide; the resolution, R, between the dimethylformamide peak and the dimethyl sulfoxide peak is not less than 2; the tailing factors for the dimethylformamide peak and the dimethyl sulfoxide peak are not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure [noteUse peak heights where peak responses are indicated. ] Separately inject equal volumes (about 2 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms for not less than 20 minutes, and measure the responses for the dimethylformamide and dimethyl sulfoxide peaks. Calculate the percentage (v/v) of C2H6OS in the portion of Topical Solution taken by the formula:
(2.5 / 1.096)10(C / V)(RU / RS)in which 1.096 is the specific gravity of dimethyl sulfoxide, C is the concentration, in mg per mL, of USP Dimethyl Sulfoxide RS in the Standard preparation; V is the volume, in mL, of Topical Solution taken to prepare the Assay preparation; and RU and RS are the ratios of the dimethyl sulfoxide peak response to the dimethylformamide peak response in the chromatograms obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 2927